[Federal Register Volume 77, Number 97 (Friday, May 18, 2012)]
[Rules and Regulations]
[Pages 29757-29846]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 2012-10210]



[[Page 29757]]

Vol. 77

Friday,

No. 97

May 18, 2012

Part II





Environmental Protection Agency





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40 CFR Parts 136, 260, et al.





Guidelines Establishing Test Procedures for the Analysis of Pollutants 
Under the Clean Water Act; Analysis and Sampling Procedures; Final Rule

Federal Register / Vol. 77 , No. 97 / Friday, May 18, 2012 / Rules 
and Regulations

[[Page 29758]]


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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 136, 260, 423, 430, and 435

[EPA-HQ-OW-2010-0192; FRL-9664-6]
RIN 2040-AF09


Guidelines Establishing Test Procedures for the Analysis of 
Pollutants Under the Clean Water Act; Analysis and Sampling Procedures

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: This rule modifies the testing procedures approved for 
analysis and sampling under the Clean Water Act. EPA proposed these 
changes for public comment on September 23, 2010. The changes adopted 
in this final rule fall into the following categories: New and revised 
EPA methods and new and revised methods published by voluntary 
consensus standard bodies (VCSB), such as ASTM International and the 
Standard Methods Committee; updated versions of currently approved 
methods; methods reviewed under the alternate test procedures (ATP) 
program; clarifications to the process for EPA approval for use of 
alternate procedures for nationwide and Regional use; minimum quality 
control requirements to improve consistency across method versions; 
corrections to previously approved methods; and revisions to sample 
collection, preservation, and holding time requirements. Finally, EPA 
makes changes to three effluent guideline regulations.

DATES: This regulation is effective on June 18, 2012. The incorporation 
by reference of these methods is approved by the Director of the 
Federal Register on June 18, 2012. For judicial review purposes, this 
final rule is promulgated as of 1:00 p.m. (Eastern time) on June 1, 
2012 as provided at 40 CFR 23.2 and 23.7.

ADDRESSES: EPA has established a docket for this action under Docket ID 
No. EPA-HQ-OW-2010-0192. All documents in the docket are listed on the 
http://www.regulations.gov Web site. Although listed in the index, some 
information is not publically available, e.g., CBI or other information 
whose disclosure is restricted by statute. Certain other materials, 
such as copyrighted material, are not placed on the Internet and will 
be publicly available only in hard copy form. Publicly available docket 
materials are available either electronically through http://www.regulations.gov or in hard copy at the HQ Water Docket Center, EPA/
DC, EPA West, Room 3334, 1301 Constitution Ave. NW., Washington, DC. 
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday 
through Friday, excluding legal holidays. The telephone number for the 
Public Reading Room is 202-566-1744, and the telephone number is 202-
566-2426 for the HQ Water Docket.

FOR FURTHER INFORMATION CONTACT: For information regarding the changes 
to inorganic chemical methods, contact Lemuel Walker, Engineering and 
Analysis Division (4303T), USEPA Office of Science and Technology, 1200 
Pennsylvania Ave. NW., Washington, DC 20460, 202-566-1077 (email: 
walker.lemuel@epa.gov). For information regarding the changes to 
organic chemical methods, contact Maria Gomez-Taylor, Engineering and 
Analysis Division (4303T), USEPA Office of Science and Technology, 1200 
Pennsylvania Ave. NW., Washington, DC 20460, 202-566-1005 (email: 
gomez-taylor.maria@epa.gov). For information regarding the changes to 
microbiological and whole effluent toxicity methods, contact Robin 
Oshiro, Engineering and Analysis Division (4303T), USEPA Office of 
Science and Technology, 1200 Pennsylvania Ave. NW., Washington, DC 
20460, 202-566-1075 (email: oshiro.robin@epa.gov).

SUPPLEMENTARY INFORMATION:

A. General Information

1. Does this action apply to me?

    EPA Regions, as well as States, Territories and Tribes authorized 
to implement the National Pollutant Discharge Elimination System 
(NPDES) program, issue permits with conditions designed to ensure 
compliance with the technology-based and water quality-based 
requirements of the Clean Water Act (CWA). These permits may include 
restrictions on the quantity of pollutants that may be discharged as 
well as pollutant measurement and reporting requirements. If EPA has 
approved a test procedure for analysis of a specific pollutant, the 
NPDES permittee must use an approved test procedure (or an approved 
alternate test procedure if specified by the permitting authority) for 
the specific pollutant when measuring the required waste constituent. 
Similarly, if EPA has established sampling requirements, measurements 
taken under an NPDES permit must comply with these requirements. 
Therefore, entities with NPDES permits will potentially be affected by 
the actions in this rulemaking. Categories and entities that may 
potentially be affected by the requirements of today's rule include:

------------------------------------------------------------------------
                                      Examples of potentially affected
             Category                             entities
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State, Territorial, and Indian      States, Territories, and Tribes
 Tribal Governments.                 authorized to administer the NPDES
                                     permitting program; States,
                                     Territories, and Tribes providing
                                     certification under Clean Water Act
                                     section 401; State, Territorial,
                                     and Indian Tribal owned facilities
                                     that must conduct monitoring to
                                     comply with NPDES permits.
Industry..........................  Facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
Municipalities....................  POTWs or other municipality owned
                                     facilities that must conduct
                                     monitoring to comply with NPDES
                                     permits.
------------------------------------------------------------------------

    This table is not intended to be exhaustive, but rather provides a 
guide for readers regarding entities likely to be affected by this 
action. This table lists types of entities that EPA is now aware of 
that could potentially be affected by this action. Other types of 
entities not listed in the table could also be affected. To determine 
whether your facility is affected by this action, you should carefully 
examine the applicability language at 40 CFR 122.1 (NPDES purpose and 
scope), 40 CFR 136.1 (NPDES permits and CWA) and 40 CFR 403.1 
(Pretreatment standards purpose and applicability). If you have 
questions regarding the applicability of this action to a particular 
entity, consult the appropriate person listed in the preceding FOR 
FURTHER INFORMATION CONTACT section.

B. What process governs judicial review of this rule?

    Under Section 509(b)(1) of the Clean Water Act (CWA), judicial 
review of today's CWA rule may be obtained by filing a petition for 
review in a United States Circuit Court of Appeals within 120 days from 
the date of promulgation of this rule. For judicial review purposes, 
this final rule is promulgated as of 1 p.m. (Eastern time) on June 1, 
2012 as provided at 40 CFR 23.2. The

[[Page 29759]]

requirements of this regulation may also not be challenged later in 
civil or criminal proceedings brought by EPA.

C. Abbreviations and Acronyms Used in the Preamble and Final Rule

AOAC: AOAC International
ASTM: ASTM International
ATP: Alternate Test Procedure
CFR: Code of Federal Regulations
CWA: Clean Water Act
EPA: Environmental Protection Agency
FLAA: Flame Atomic Absorption Spectroscopy
HRGC: High Resolution Gas Chromatography
HRMS: High Resolution Mass Spectrometry
ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy
ICP/MS: Inductively Coupled Plasma-Mass Spectrometry
ISO: International Organization for Standardization
MS: Mass Spectrometry
NIST: National Institute of Standards and Technology
NPDES: National Pollutant Discharge Elimination System
QA: Quality Assurance
QC: Quality Control
SDWA: Safe Drinking Water Act
SM: Standard Methods
SRM: Standard Reference Material
STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption 
Spectroscopy
USGS: United States Geological Survey
VCSB: Voluntary Consensus Standards Body
WET: Whole Effluent Toxicity

Table of Contents

I. Statutory Authority
II. Summary of Final Rule
    A. New EPA Methods and New Versions of Previously Approved EPA 
Methods
    B. New Standard Methods and New Versions of Approved Standard 
Methods
    C. New ASTM Methods and New Versions of Previously Approved ASTM 
Methods
    D. New Alternate Test Procedures at 40 CFR 136.3
    E. Clarifications and Corrections to Previously Approved Methods 
in 40 CFR 136.3
    F. Revisions in Table II at 40 CFR 136.3(e) to Required 
Containers, Preservation Techniques, and Holding Times
    G. Revisions to 40 CFR 136.4 and 136.5
    H. Revisions to Method Modification Provisions at 40 CFR 136.6
    I. New Quality Assurance and Quality Control Language at 40 CFR 
136.7
    J. Revisions to 40 CFR part 423 (Steam Electric Power Generating 
Point Source Category)
III. Changes Between the Proposed Rule and the Final Rule
    A. EPA Is Not Adding EPA Method 1614A
    B. Deferral of Action on EPA Method 1668C
    C. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09
    D. Revisions and Clarifications to EPA Method 200.7
    E. Revisions and Corrections to Certain Citations in Tables IB 
and ID
    F. Continued Approval of Method 1664 Revision A
    G. Revision to Footnote 63 of Table IB at 40 CFR 136.3
    H. Revision to Footnote 4 of Table IC at 40 CFR 136.3
    I. Revisions to Table II Language
    J. Approval of Alternate Test Procedures for Limited Use at 40 
CFR 136.5
    K. Revisions to Language at Sec.  136.6
    L. Revisions to New Quality Assurance and Quality Control 
Language
    M. Withdrawal of Appendices at 40 CFR part 136
    N. Revisions to 40 CFR Part 430 (Pulp, Paper, and Paperboard 
Point Source Category)
    O. Revisions to 40 CFR Part 435 (Oil and Gas Extraction Point 
Source Category)
IV. Response to Comments
    A. How Standard Methods are Identified in Part 136 Tables
    B. Preservation and Holding Time Requirements for EPA Method 624
    C. Quality Assurance and Quality Control Requirements
V. Statutory and Executive Order Reviews
    A. Executive Order 12866: Regulatory Planning and Review and 
Review and Executive Order 13563: Improving Regulation and 
Regulatory Review
    B. Paperwork Reduction Act
    C. Regulatory Flexibility Act
    D. Unfunded Mandates Reform Act
    E. Executive Order 13132: Federalism
    F. Executive Order 13175: Consultation and Coordination With 
Indian Tribal Governments
    G. Executive Order 13045: Protection of Children From 
Environmental Health Risks and Safety Risks
    H. Executive Order 13211: Actions That Significantly Affect 
Energy Supply, Distribution, or Use
    I. National Technology Transfer and Advancement Act of 1995
    J. Executive Order 12898: Federal Actions To Address 
Environmental Justice in Minority Populations and Low-Income 
Populations
    K. Congressional Review Act

I. Statutory Authority

    EPA is promulgating today's rule pursuant to the authority of 
sections 301(a), 304(h), and 501(a) of the Clean Water Act (``CWA'' or 
the ``Act''), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of 
the Act prohibits the discharge of any pollutant into navigable waters 
unless the discharge complies with a National Pollutant Discharge 
Elimination System (NPDES) permit issued under section 402 of the Act. 
Section 304(h) of the Act requires the Administrator of the EPA to ``* 
* * promulgate guidelines establishing test procedures for the analysis 
of pollutants that shall include the factors which must be provided in 
any certification pursuant to [section 401 of this Act] or permit 
application pursuant to [section 402 of this Act].'' Section 501(a) of 
the Act authorizes the Administrator to ``* * * prescribe such 
regulations as are necessary to carry out this function under [the 
Act].'' EPA generally has codified its test procedure regulations 
(including analysis and sampling requirements) for CWA programs at 40 
CFR part 136, though some requirements are codified in other Parts 
(e.g., 40 CFR Chapter I, Subchapters N and O).

II. Summary of Final Rule

    The following sections describe the changes EPA is making in 
today's final rule.

A. New EPA Methods and New Versions of Previously Approved EPA Methods

    This rule approves new EPA methods and new versions of already 
approved EPA methods. The following discussion briefly describes the 
EPA methods added today to Part 136.
    1. Oil and grease. Today's rule adds a new version of EPA Method 
1664, 1664 Revision B: n-Hexane Extractable Material (HEM; Oil and 
Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; 
Non-polar Material) by Extraction and Gravimetry for use in CWA 
programs. Today, EPA is also amending the RCRA regulations at 40 CFR 
260.11, which currently specify the use of Method 1664 Rev. A, to 
provide additionally for use of the revised version, 1664 Rev. B. As 
stated in the preamble to the proposal (75 FR 58026, Sept. 23, 2010), 
EPA encourages that future delistings cite ``Method 1664 Rev. B'' while 
delistings already granted may continue to use Method 1664 Rev. A.
    On December 14, 2011, EPA published a notice of data availability 
(NODA) on a new method for oil and grease for use in Clean Water Act 
programs (see 76 FR 77742). This method, ASTM D-7575-10, uses a 
different extractant (a membrane filter instead of n-hexane for the 
extraction of oil and grease material) and a different measurement 
technique (infrared absorption instead of gravimetry) from the 
extractant and measurement technique of currently approved methods for 
oil and grease. The new method was discussed in the September 23, 2010 
notice but EPA did not propose it for use as an approved method to be 
codified at 40 CFR 136.3 because oil and grease is a method-defined 
parameter. By definition, the measurement results of method-defined 
parameters are specific to the described method and are not directly 
comparable to results obtained by another method. However, since 
publication of the Methods Update Rule proposal, the Agency received 
additional data and information about this method and is re-considering 
whether it should add this

[[Page 29760]]

method to the list of approved methods for oil and grease at 40 CFR 
136.3. In the NODA, EPA proposed to include ASTM D-7575 for the 
measurement of oil and grease based on comments received in response to 
its September 23, 2010 proposal and the additional data. EPA will make 
a decision on the inclusion of the new method once it reviews the 
public comments received in response to the NODA and will then publish 
that decision in a separate Federal Register notice.
    2. Metals. Today's rule adds EPA Method 200.5 (Revision 4.2): 
``Determination of Trace Elements in Drinking Water by Axially Viewed 
Inductively Coupled Plasma--Atomic Emission Spectrometry'' to Table IB. 
The rule also clarifies that the axial orientation of the torch is 
allowed for use with EPA Method 200.7. Thus, EPA will allow the use of 
axial instruments or radial instruments to measure metals in water 
samples.
    3. Pesticides. Today's rule adds EPA Method 525.2 to Table IG (Test 
Methods for Pesticide Active Ingredients) as an additional approved 
method for all parameters for which EPA has previously approved EPA 
Method 525.1, and also adds Methods 525.1 and 525.2 to Table ID for the 
same parameters for which EPA had previously approved Method 525.1 in 
Table IG. The rule also adds some of the methods for Pesticide Active 
Ingredients (Table IG) to applicable parameters listed in Table ID for 
general use. These methods are:
    a. EPA Method 608.1, ``The Determination of Organochlorine 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures chlorobenzilate, chloroneb, chloropropylate, 
dibromochloropropane, etridiazole, PCNB, and propachlor.
    b. EPA Method 608.2, ``The Determination of Certain Organochlorine 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures chlorothalonil, DCPA, dichloran, methoxychlor, and permethrin.
    c. EPA Method 614, ``The Determination of Organophosphorus 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures azinphos methyl, demeton, diazinon, disulfoton, ethion, 
malathion, parathion methyl, and parathion ethyl.
    d. EPA Method 614.1, ``The Determination of Organophosphorus 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures dioxathion, EPN, ethion, and terbufos.
    e. EPA Method 615, ``The Determination of Chlorinated Herbicides in 
Municipal and Industrial Wastewater.'' This method measures 2,4-D, 
dalapon, 2,4-DB, dicamba, dichlorprop, dinoseb, MCPA, MCPP, 2,4,5-T, 
and 2,4,5-TP.
    f. EPA Method 617, ``The Determination of Organohalide Pesticides 
and PCBs in Municipal and Industrial Wastewater.'' This method measures 
aldrin, [alpha]-BHC, [beta]-BHC, [gamma]-BHC (lindane), captan, 
carbophenothion, chlordane, 4,4'-DDD, 4,4'-DDE, 4,4'-DDT, dichloran, 
dicofol, dieldrin, endosulfan I, endosulfan II, endosulfan sulfate, 
endrin, endrin aldehyde, heptachlor, heptachlor epoxide, isodrin, 
methoxychlor, mirex, PCNB, perthane, strobane, toxaphene, trifluralin, 
PCB-1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254, and PCB-
1260.
    g. EPA Method 619, ``The Determination of Triazine Pesticides in 
Municipal and Industrial Wastewater.'' This method measures ametryn, 
atraton, atrazine, prometon, prometryn, propazine, sec-bumeton, 
simetryn, simazine, terbuthylazine, and terbutryn.
    h. EPA Method 622, ``The Determination of Organophosphorus 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures azinphos methyl, bolstar, chlorpyrifos, chlorpyrifos methyl, 
coumaphos, demeton, diazinon, dichlorvos, disulfoton, ethoprop, 
fensulfothion, fenthion, merphos, mevinphos, naled, parathion methyl, 
phorate, ronnel, stirofos, tokuthion, and trichloronate.
    i. EPA Method 622.1, ``The Determination of Thiophosphate 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures aspon, dichlofenthion, famphur, fenitrothion, fonophos, 
phosmet, and thionazin.
    j. EPA Method 632, ``The Determination of Carbamate and Urea 
Pesticides in Municipal and Industrial Wastewater.'' This method 
measures aminocarb, barban, carbaryl, carbofuran, chlorpropham, diuron, 
fenuron, fenuron-TCA, fluometuron, linuron, methiocarb, methomyl, 
mexacarbate, monuron, monuron-TCA, neburon, oxamyl, propham, propoxur, 
siduron, and swep.
    4. Microbiologicals. Today's rule approves the 2005 versions of EPA 
Method 1622, ``Cryptosporidium in Water by Filtration/IMS/FA'' and EPA 
Method 1623, ``Cryptosporidium and Giardia in Water by Filtration/IMS/
FA'' in Table IH for ambient water.
    The rule approves revised versions of EPA Methods 1103.1, 1106.1, 
1600, 1603, and 1680 in Table IH. The rule also approves the revised 
version of EPA Methods 1600, 1603 and 1680 in Table IA. We corrected 
technical errors in these revisions.
    5. Non-Conventionals. Today's rule adds EPA Method 1627, ``Kinetic 
Test Method for the Prediction of Mine Drainage Quality'' to Table IB 
as a new parameter termed ``Acid Mine Drainage.''
    6. Organics. Today's rule approves EPA Method 624, ``Purgeables,'' 
for the determination of acrolein and acrylonitrile in wastewater and 
revises footnote 4 to Table IC to specify that the laboratory must 
provide documentation about its ability to measure these analytes at 
the levels necessary to comply with associated regulations.

B. New Standard Methods and New Versions of Approved Standard Methods

    This rule approves the following Standard Methods (SM) for certain 
pollutants currently listed in Table IB at Part 136. Laboratories 
performing measurements using any of the approved Standard Methods must 
follow the quality control (QC) procedures specified in the 20th or 
21st edition of Standard Methods. Below is a list of the Standard 
Methods added to Table IB in Part 136:

1. SM 5520 B-2001 and SM 5520 F-2001, Oil and Grease, gravimetric
2. SM 4500-NH3 G-1997, Ammonia (as N) and TKN, automated 
phenate method
3. SM 4500-B B-2000, Boron, curcumin method
4. SM 4140 B-1997, Inorganic Ions (Bromide, Chloride, Fluoride, 
Orthophosphate, and Sulfate), capillary ion electrophoresis with 
indirect UV detection
5. SM 3114 B-2009, Arsenic and Selenium, AA gaseous hydride
6. SM 3114 C-2009, Arsenic and Selenium, AA gaseous hydride
7. SM 3111 E-1999, Aluminum and Beryllium, direct aspiration atomic 
absorption spectrometry
8. SM 5220 B-1997, Chemical Oxygen Demand (COD), titrimetric
9. SM 3500-Cr B-2009, Chromium, colorimetric method
10. SM 4500-Norg D-1997, Kjeldahl Nitrogen, semi-automated 
block digestor colorimetric
11. SM 3112 B-2009, Mercury, cold vapor, manual
12. SM 4500-P G-1999 and SM 4500-P H-1999, Phosphorus, Total, automated 
ascorbic acid reduction
13. SM 4500-P E-1999 and SM 4500-P F-1999, Phosphorus, Total, manual, 
and automated ascorbic acid reduction
14. SM 4500-O B, D, E and F-2001, Oxygen, Dissolved, Winkler
15. SM 4500-O D-2001, Oxygen, Dissolved, Winkler

[[Page 29761]]

16. SM 4500-O E-2001, Oxygen, Dissolved, alum flocculation modification
17. SM 5530 B-2005, Phenols, manual distillation
18. SM 5530 D-2005, Phenols, colorimetric
19. SM 3500-K C-1997, Potassium, Total, selective electrode method
20. SM 2540 E-1997, Residues--Volatile, gravimetric
21. SM 4500-SiO2 E-1997 and SM 4500-SiO2 F-1997, 
Silica, Dissolved, automated molybdosilicate
22. SM 4500-SO42- C-1997, D-1997, E-1997, F-1997 
and G-1997, Sulfate, gravimetric, and automated colorimetric
23. SM 4500-S2- B-2000 and C-2000, Sulfide, sample 
pretreatment

 C. New ASTM Methods and New Versions of Previously Approved ASTM 
Methods

    The rule approves the following ASTM methods for existing 
pollutants and ASTM methods for new pollutants to 40 CFR part 136, 
Table IB for inorganic compounds, and Table IC for organic compounds.
1. ASTM D2036-09 (B), Cyanide--Total, Cyanide amenable to cholorination
2. ASTM D6888-09, Cyanide--Available, flow injection and ligand 
exchange
3. ASTM D7284-08, Cyanide--Total, flow injection
4. ASTM D7511-09, Cyanide--Total, segmented flow injection
5. Free cyanide is added as a new parameter (24A in Table IB); two ASTM 
methods (D4282-02 and D7237-10) are approved, in addition to a new 
version of OIA 1677(2009) for this parameter. D4282-02 is a Standard 
Test Method for Determination of Free Cyanide in Water and Wastewater 
by Microdiffusion, and Method D7237-10 is a Standard Test Method for 
Free Cyanide with Flow Injection Analysis (FIA) Utilizing Gas Diffusion 
Separation and Amperometric Detection.
6. ASTM D888-09 (A), Oxygen Dissolved, Winkler
7. ASTM D7573-09, Organic Carbon--Total, combustion
8. ASTM D7065-06, Five new chemicals in water: Nonylphenol (NP), 
Bisphenol A (BPA), p-tert-Octylphenol (OP), Nonylphenol Monoethoxylate 
(NP1EO), and Nonylphenol Diethoxylate (NP2EO), Gas Chromatography/Mass 
Spectrometry

D. New Alternate Test Procedures at 40 CFR 136.3

The rule approves eight methods submitted to EPA for review through the 
alternate test procedures (ATP) program and deemed acceptable based on 
the evaluation of documented method performance. The eight methods 
approved are added to Table IB:

1. Hach Company's Method 10360 Luminescence Measurement of Dissolved 
Oxygen in Water and Wastewater and for Use in the Determination of 
BOD5 and cBOD5, Revision 1.2 dated October 2011
2. In-Situ Incorporated's Method 1002-8-2009 Dissolved Oxygen 
Measurement by Optical Probe
3. In-Situ Incorporated's Method 1003-8-2009 Biochemical Demand (BOD) 
Measurement by Optical Probe
4. In-Situ Incorporated's Method 1004-8-2009 Carbonaceous Biochemical 
Oxygen Demand (CBOD) Measurement by Optical Probe
5. Mitchell Method M5271 dated July 31, 2008 for turbidity
6. Mitchell Method M5331 dated July 31, 2008 for turbidity
7. Thermo Scientific's Orion Method AQ4500 dated March 12, 2009 for 
turbidity
8. Easy (1-Reagent) Nitrate Method dated November 12, 2011 for nitrate, 
nitrite and combined nitrate/nitrite

E. Clarifications and Corrections to Previously Approved Methods in 40 
CFR 136.3

    The rule also clarifies the procedures for measuring orthophosphate 
and corrects typographical or other citation errors in Part 136. 
Specifically, the rule clarifies the purpose of the immediate 
filtration requirement in orthophosphate measurements (Table IB, 
parameter 44), which is to assess the dissolved or bio-available form 
of orthophosphorus (i.e., that portion which passes through a 0.45-
micron filter)--hence the requirement to filter the sample immediately 
upon collection (i.e., within 15 minutes of collection). EPA has added 
a footnote (24) to Table II providing this clarification. The rule also 
corrects missing citations to the table of microbiological methods for 
ambient water monitoring which are specified in Table IH at 40 CFR 
136.3. When EPA approved the use of certain microbiological methods on 
March 26, 2007 (72 FR 14220), EPA inadvertently omitted fecal coliform, 
total coliform, and fecal streptococcus methods from the table. This 
omission is corrected in today's rule.

F. Revisions in Table II at 40 CFR 136.3(e) to Required Containers, 
Preservation Techniques, and Holding Times

    The rule revises some of the current requirements in Table II at 
136.3(e).
    1. The rule revises footnote 4 of Table II to clarify the sample 
holding time for the Whole Effluent Toxicity (WET) samples for the 
three toxicity methods by adding the following sentence: ``For static-
renewal toxicity tests, each grab or composite sample may also be used 
to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after 
first use, if stored at 0-6 [deg]C, with minimum head space.'' In 
addition, EPA will post on the WET Web site corrections to errata in 
the ``Short-term Methods for Estimating the Chronic Toxicity of 
Effluents and Receiving Waters to Freshwater Organisms'' manual (EPA 
2010e).
    2. The rule revises the cyanide sample handling instructions in 
Footnote 5 of Table II to recommend the treatment options for samples 
containing oxidants described in ASTM's sample handling practice for 
cyanide samples, D7365-09a.
    3. The rule revises the cyanide sample handling instructions in 
Footnote 6 of Table II to describe options available when the 
interference mitigation instructions in D7365-09a are not effective, 
and to allow the use of any technique for removal or suppression of 
interference, provided the laboratory demonstrates and documents that 
the alternate technique more accurately measures cyanide through 
quality control measures described in the analytical test method.
    4. The rule revises footnote 16 of Table II instructions for 
handling Whole Effluent Toxicity (WET) samples by adding two sentences: 
``Aqueous samples must not be frozen. Hand-delivered samples used on 
the day of collection do not need to be cooled to 0 to 6 [deg]C prior 
to test initiation.''
    5. The rule revises footnote 22 to Table II to read ``Sample 
analysis should begin as soon as possible after receipt; sample 
incubation must be started no later than 8 hours from time of 
collection.''
    6. The rule adds three entries at the end of Table II with the 
containers, preservation, and holding times for the alkylated phenols, 
adsorbable organic halides, and chlorinated phenolics. When EPA 
proposed ASTM D7065-06 for the alkylated phenols, commenters noted that 
EPA did not include preservation and holding time information in Table 
II. When EPA moved EPA Methods 1650 and 1653

[[Page 29762]]

from 40 CFR part 430 to Table IC, EPA inadvertently omitted the 
associated parameters to Table II, and is correcting this omission in 
today's rule. The Table II information for containers, preservation, 
and holding times for these three new entries are taken from the 
approved methods.

G. Revisions to 40 CFR 136.4 and 136.5

    This rule changes Sec. Sec.  136.4 and 136.5 to clarify the 
procedures for obtaining review and approval for the use of alternate 
test procedures (alternate methods or ATPs) for those methods for which 
EPA has published an ATP protocol (there are published protocols for 
chemistry, radiochemical, and microbiological culture methods). In 
particular, it establishes separate sections outlining the procedures 
for obtaining EPA review and approval for nationwide use of an ATP 
(Sec. Sec.  136.4), and the procedures for obtaining approval for 
limited use of an ATP (Sec. Sec.  136.5).
    In addition, this rule adds language to Part 136.5 to clarify the 
purpose and intent of limited use applications. This provision only 
allows use of an alternate method for a specific application at a 
facility or type of discharge. The Regional Alternate Test Procedure 
(ATP) Coordinator or the permitting authority, at his/her discretion, 
may grant approval to all discharges or facilities specified in the 
approval letter. However, the appropriate permitting authority within a 
state may request supporting test data from each discharger or facility 
prior to allowing any such approvals.
    Today's rule further clarifies that the limited use provision 
cannot be used to gain nationwide approval and is not a way to avoid 
the full examination of comparability that is required for alternate 
test procedures when EPA considers a method for nationwide use with the 
ultimate goal of listing it as an approved CWA method at 40 CFR part 
136. As further clarification, in the event that EPA decides not to 
approve a method proposed for nationwide use, the Regional ATP 
Coordinator or the permitting authority may choose to reconsider any 
previous limited use approvals of the alternate method. Based on this 
reconsideration, the Regional ATP Coordinator or the permitting 
authority will notify the user(s) if the limited use approval is 
withdrawn. Otherwise, the limited use approvals remain in effect.

H. Revisions to Method Modification Provisions at 40 CFR 136.6

    This section allows users to make certain modifications to an 
approved method to address matrix interferences without the extensive 
review and approval process specified for an alternate test procedure 
at 136.4 and 136.5. Today's rule revises 136.6 to provide more examples 
of allowed and prohibited method modifications. The intent of today's 
revisions is to clarify those situations in which an ATP is required 
and those where it is not. Analysts may use the examples to help assess 
the need for a formal ATP, and in the event an ATP is not needed to 
document that their modification is acceptable and does not depart 
substantially from the chemical principles in the method being 
modified.
    In response to comments, EPA has included additional examples of 
allowed and prohibited method modifications and has made some revisions 
to the text language as discussed in Section III below.

I. New Quality Assurance and Quality Control Language at 40 CFR 136.7

    EPA is specifying ``essential'' quality control elements at Sec.  
136.7 for use in conducting an analysis for CWA compliance monitoring. 
This new language is added because auditors, co-regulators, laboratory 
personnel, and the regulated community have noted the variations in 
quality assurance (QA) and quality control (QC) procedures practiced by 
laboratories that use 40 CFR part 136 methods for compliance 
monitoring. Some of these methods are published by voluntary consensus 
standards bodies, such as the Standard Methods Committee, and ASTM 
International. Standard Methods and ASTM are available in printed or 
electronic compendia, or as individual online files. As mentioned in 
the proposal, each organization has a unique compendium structure. QA 
and QC method guidance or requirements may be listed directly in the 
approved consensus method, or, as is more often the case, these 
requirements are listed in other parts of the compendium.
    Regardless of the publisher, edition, or source of an analytical 
method approved for CWA compliance monitoring, analysts must use 
suitable QA/QC procedures whether EPA or other method publishers have 
specified these procedures in a particular Part 136 method, or 
referenced these procedures by other means. These records must be kept 
in-house as part of the method testing documentation. Consequently, 
today's rule clarifies that an analyst using these consensus standard 
body methods for reporting under the CWA must also comply with the 
quality assurance and quality control requirements listed in the 
appropriate sections in that consensus standard body compendium. EPA's 
approval of use of these voluntary consensus standard body methods 
contemplated that any analysis using such methods would also meet the 
quality assurance and quality control requirements prescribed for the 
particular method. Thus, not following the applicable and appropriate 
quality assurance and quality control requirements of the respective 
method means that the analysis does not comply with the requirements in 
EPA's NPDES regulations to monitor in accordance with the procedures of 
40 CFR part 136 for analysis of pollutants.
    For methods that lack QA/QC requirements (as specified in this new 
section at 40 CFR 136.7), whether developed by EPA, a vendor, or a 
consensus standard body, analysts can refer to and follow the QA/QC 
published in several public sources. Examples of these sources include 
the relevant QA/QC sections of an equivalent approved EPA method, or 
voluntary consensus standards published as Part 136 approved methods 
(e.g., Standard Methods, ASTM International, and AOAC). In addition to 
and regardless of the source of the laboratory's or method's QA and QC 
instructions, for methods that lack QA/QC requirements, EPA is adding 
requirements at 136.7 to specify twelve essential quality control 
elements that must be in the laboratory's documented quality system 
unless a written rationale is provided to explain why these quality 
control elements are inappropriate for a specific analytical method or 
application. These twelve essential quality control checks must be 
clearly documented in the written SOP (or method) along with a 
performance specification or description for each of the twelve checks, 
as applicable to the specific method. EPA has clarified the language in 
this section in response to public comments. The revised language is 
discussed in section III below.

J. Revisions at 40 CFR Part 423 (Steam Electric Power Generating Point 
Source Category)

    The rule revises the 40 CFR part 423 definitions for total residual 
chlorine and free available chlorine at Sec. Sec.  423.11(a) and 
423.11(l) to allow the use of ``chlorine--total residual'' and 
``chlorine--free available'' methods in Sec.  136.3(a), Table IB, or 
other methods approved by the permitting authority.

[[Page 29763]]

III. Changes Between the Proposed Rule and the Final Rule

    Except as noted below, the content of the final rule is the same as 
that of the proposed rule.

A. EPA Is Not Adding EPA Method 1614A

    The Agency proposed to add Method 1614A, ``Brominated Diphenyl 
Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS.'' EPA 
developed this method to determine 49 polybrominated diphenyl ether 
(PBDE) congeners in aqueous, solid, tissue, and multi-phase matrices. 
This method uses isotope dilution and internal standard high resolution 
gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The 
commenters were divided on whether EPA should approve this method. Two 
commenters stated that Method 1614A would be a valuable addition to the 
list of approved methods, while two other commenters stated that the 
method has not been sufficiently validated for use in Clean Water Act 
programs. Upon further evaluation of the data supporting the use of 
this test procedure and the peer review comments, EPA agrees with those 
commenters who stated that additional validation data are needed to 
fully characterize the performance of this method for various matrices 
and has decided not to include Method 1614A in today's final rule.

B. Deferral of Action on EPA Method 1668C

    The Agency proposed to add EPA Method 1668C, ``Chlorinated Biphenyl 
Congeners in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/
HRMS.'' This method measures individual chlorinated biphenyl congeners 
in environmental samples by isotope dilution and internal standard high 
resolution gas chromatography/high resolution mass spectrometry (HRGC/
HRMS). As discussed in the proposal, Part 136 methods for chlorinated 
biphenyls (PCBs) only measure a mixture of congeners in seven 
Aroclors--PCB-1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254, 
and PCB-1260, while Method 1668C can measure the 209 PCB congeners in 
these mixtures.
    EPA began development of this method in 1995, initially covering 13 
congeners labeled ``toxic'' by the World Health Organization. In 1999, 
EPA expanded the scope of the method to include all 209 PCB congeners. 
The method has been used to support several studies, including the 2001 
National Sewage Sludge Survey and the National Lake Fish Tissue Survey. 
Since 1999, EPA has revised the method to incorporate additional 
information and data collected such as the results of an inter-
laboratory validation study, peer reviews of the method and the 
validation study data, additional QC performance criteria and MDL data, 
and user experiences. In the development and subsequent multi-
laboratory validation of this method, EPA evaluated method performance 
characteristics, such as selectivity, calibration, bias, precision, 
quantitation and detection limits. The Agency is aware that this method 
is being used in some states in their regulatory programs and by other 
groups for some projects with good success. For example, in a study of 
data comparability between two laboratories on samples collected from 
the Passaic River in New Jersey, in which 151 PCB congeners were 
identified and measured, accuracy, as measured by analysis of an NIST 
SRM, was 15% or better. Recoveries of the PCB congeners ranged from 90% 
to 124% and averaged 105%; precision ranged from 4.2 to 23% (Passaic 
River 2010). This type of data shows that recoveries and precision for 
this method are within the performance achievable with other approved 
methods.
    EPA received comments from thirty-five individuals or organizations 
on this method. Of these commenters, five (three states, one 
laboratory, and one laboratory organization) supported the approval of 
this method. Some states indicated that they are already requiring this 
method for use in permits and for other purposes. On the other hand, 
industry and industry groups/associations were critical of the method 
for various reasons. Commenters opposing the method provided a detailed 
critique of the method, the inter-laboratory study, the peer reviews 
and the other supporting documentation. Among the criticisms of the 
inter-laboratory study, commenters argued that: (1) EPA did not produce 
documentation supporting changes to the method approved by EPA for the 
interlaboratory study, (2) the raw data for wastewater and biosolids 
was poor and is not fit for use in a comprehensive interlaboratory 
study, (3) EPA cited certain guidelines such as ASTM but deviated from 
those guidelines (e.g., used only one Youden pair per matrix), (4) the 
peer reviewers' qualifications were questioned, (5) the addendum and 
the pooled MDLs/MLs were not subjected to peer review, (6) MDL/ML are 
flawed, the process to calculate MDLs/MLs for congeners that co-elute 
was flawed, the MDL/ML ignored the ubiquitous problem of background 
contamination, and (7) the validation study did not include all 
matrices in the method (soil and sediment excluded). In addition, some 
commenters also suggested that EPA should first promulgate new 
detection and quantitation procedures. Further, commenters raised 
questions about possible adverse effects of this new method on 
compliance monitoring as well as concerns about data reporting and 
costs.
    EPA is still evaluating the large number of public comments and 
intends to make a determination on the approval of this method at a 
later date. In the meantime, the Agency has decided to go forward with 
the promulgation of the other proposed analytical methods to expedite 
their implementation by the regulated community and laboratories. This 
decision does not negate the merits of this method for the 
determination of PCB congeners in regulatory programs or for other 
purposes when analyses are performed by an experienced laboratory.

C. EPA Is Not Adding ASTM Methods D7574-09 and D7485-09

    In today's rule, EPA is not adding two proposed ASTM methods, ASTM 
D7574-09 ``Standard Test Method for Determination of Bisphenol A 
(BPA),'' and ASTM D7485-09 ``Standard Test Method for Determination of 
NP, OP, NP1EO, and NP2EO.'' These two methods involve liquid 
chromatography and tandem mass spectrometry (LC/MS/MS). The methods 
have been tested by a single laboratory in several environmental 
waters, and may be useful for many applications. However, EPA has 
decided to postpone approval of these two methods for general use until 
completion of a full inter-laboratory validation study designed to 
fully characterize the performance of these methods across multiple 
laboratories and matrices.

D. Revisions and Clarifications to EPA Method 200.7

    EPA Method 200.5 ``Determination of Trace Elements in Drinking 
Water by Axially Viewed Inductively Coupled Plasma--Atomic Emission 
Spectrometry'' employs a plasma torch viewed in the axial orientation 
to measure chemical elements (metals). As stated earlier in today's 
rule, EPA is adding Method 200.5 for some metals in Table IB. Both 
Methods 200.5 and 200.7 are acceptable methods under Part 136 and both 
methods employ ICP/AES technology. However, Method 200.5 includes 
performance data for the axial configuration that is not in Method 
200.7 because the axial technology torch

[[Page 29764]]

results were not available when Method 200.7 was developed. For some 
parameters listed in Table IB, the axial orientation using ICP/AES 
technology results in greater sensitivity and lower detection limits 
than the radial orientation. Thus, today's approval of Method 200.5 and 
the additional flexibility to modify Method 200.7 to use the axial 
orientation discussed in the proposal will allow laboratories to use 
either axial instruments or radial instruments to measure metals in 
water samples with Method 200.7. In response to EPA's proposal to allow 
the use of the axial orientation of the torch with EPA Method 200.7, 
commenters expressed support for this added flexibility. Thus, today's 
rule clarifies that the use of the axial orientation of the torch to 
measure metals is an acceptable modification to Method 200.7. EPA has 
added new text at Part 136.6(b)(5) to allow the use of the axial 
orientation of the torch for Method 200.7 as an acceptable method 
modification that does not require an ATP application.
    EPA further notes that there was a typographical error in Section 
II.J of the proposed rule which stated that the version of EPA Method 
200.7 (which the Agency proposed to remove; with Appendix C, see 
section IIIM below) has been superseded by Revision 5.4 of Method 
200.7. Today's final rule reflects that the correct reference is 
Revision 4.4 of EPA Method 200.7. In today's rule, EPA has added Method 
200.7 Revision 4.4 as an additional approved method for the measurement 
of titanium. As some commenters pointed out, EPA Method 200.7 covers 
this parameter and exclusion of this method for the measurement of 
titanium in Table IB was an oversight.
    In addition, EPA has removed EPA Method 200.7 from Table IB for the 
measurement of mercury. The addition of EPA Method 200.7 to the list of 
approved methods for mercury in Table IB was an error. Although this 
pollutant is on the list of analytes in EPA Method 200.7, mercury may 
be lost to the atmosphere through the use of the approved total 
recoverable metals digestion procedures (e.g., EPA Method 200.2, or the 
digestion procedures listed in EPA Method 200.7) that must be applied 
to the wastewater samples of interest under the Clean Water Act 
program. Such losses can lead to poor recovery in the samples compared 
to the sample preparation procedures included in other mercury methods 
approved at 40 CFR part 136. Therefore, EPA Method 200.7 has not been 
included in Table IB for mercury.

E. Revisions and Corrections to Certain Citations in Tables IA, IB, IC, 
ID, and IG

    EPA proposed some additions to Table IB which include some new 
Standard Methods or new versions of approved Standard Methods. Today's 
rule revises the applicability of some methods and makes some 
corrections to the method citations. Specifically, EPA removed SM 3120 
and SM 3125 for the measurement of mercury because mercury is not on 
the list of analytes for these methods. In addition, EPA corrected the 
citation of SM 3113 to SM 3113B-2004 in the final rule and has added SM 
3113B-2004 for the measurement of cadmium, chromium, iron, lead, and 
silver, because these analytes are covered by the method and they 
exhibit acceptable analytical performance. These omissions were an 
oversight.
    EPA also deleted from Table ID an EPA GC/MS method, Method 525.1, 
for the measurement of ametryn, diazinon, disulfoton, prometon, and 
trifluoralin. These analytes are not listed within the scope of this 
method and their inclusion in the proposal was an error.
    EPA has corrected a number of typographical errors in the tables 
and footnotes, correcting spelling and method availability information, 
method title names, and document identification numbers. A complete 
list of these changes has been included in a memo to the docket.

F. Continued Approval of Method 1664 Rev. A

    EPA proposed to replace Method 1664 Rev. A for the measurement of 
oil and grease with a revised version (Method 1664 Rev. B). This new 
version of the method describes modifications that are allowed and 
modifications that are not allowed when using this method for 
compliance with Clean Water Act regulations. Comments were generally 
supportive of the revised method but some commenters recommended that 
Method 1664 Rev. A not be withdrawn immediately because many permits 
currently specify the use of this method. In response to these 
comments, EPA will continue to allow the use of Method 1664 Rev. A for 
current permits because this method is not significantly different from 
the revised version of the method. However, EPA strongly encourages the 
use of the revised method (Method 1664 Rev. B) in the future. EPA may 
revisit this decision in a future rulemaking.

G. Revision to Footnote 63 of Table IB at 40 CFR 136.3

    EPA received comments that the Hach Method 10360, described in 
footnote 63 of Table IB, is a dissolved oxygen procedure, and as such, 
should only be listed as a procedure for dissolved oxygen, and not for 
BOD and CBOD. EPA disagrees with these commenters because the method on 
its face is clearly applicable to dissolved oxygen measurements in 
conjunction with BOD and CBOD analyses, as described in the method. As 
a result, in today's final rule, EPA added language to the end of this 
footnote to clarify that Part 136 allows the use of Hach Method 10360 
for measurement of dissolved oxygen in conjunction with the methods 
approved for measurement of biochemical demand (BOD) and carbonaceous 
biochemical oxygen demand (CBOD).

H. Revision to Footnote 4 of Table IC at 40 CFR 136.3

    EPA received comments on the proposed approval of Method 624 for 
the definitive determination of acrolein and acrylonitrile. Commenters 
agreed with the addition of these two analytes, but one of these 
commenters expressed concern about a blanket approval without requiring 
a demonstration of adequate performance and appropriate sample 
introduction techniques. This commenter recommended that performance 
criteria and information about appropriate sample introduction 
techniques be added to footnote 4 of Table IC. EPA agrees with this 
commenter's suggestions because this requirement would ensure that the 
laboratory has the ability to measure these analytes at the levels 
necessary to comply with any associated regulations. In response to 
these concerns, in today's rule, the Agency revised the footnote to add 
a statement requiring documentation of the ability to quantitatively 
measure these analytes and advising analysts that other sample 
introduction techniques may be required to achieve adequate 
performance.

I. Revisions to Table II Language

    EPA proposed to revise the text at 136.3(e) to allow any party to 
modify sample preservation and holding times after submitting 
documentation to its permitting or other authority that supports use of 
an alternative approach. Commenters expressed concern that this change 
would present a burden both to permitting authorities to review and 
approve changes, and for laboratories that work in different states 
because each state could have different requirements. In response to 
public comments, EPA has removed the proposed language at 136.3(e) that 
would have allowed such modifications based on documentation and 
procedures

[[Page 29765]]

determined by individual permitting authorities. Instead, such 
modifications must continue to be requested via a limited use ATP 
application to the Regional Alternate Test Procedure Coordinator or 
permitting authority, as appropriate. Thus, approval of any changes in 
sample preservation procedures, container materials, and maximum 
allowable holding time will remain unchanged and continue to be the 
responsibility of EPA through its Alternate Test Procedure program. EPA 
clarified language regarding the limited use application process 
procedure. Additionally, in today's rule, EPA added a clarifying 
sentence at the end of the current language to emphasize that an 
analyst cannot modify any sample preservation or holding time 
requirements in an approved method unless the requirements in Section 
136.3(e) are met.
    EPA also revised footnote 4 to Table II to delete the parenthetical 
statement specifying that samples analyzed for fecal coliforms may be 
held up to six hours prior to commencing analysis. That statement in 
footnote 4 is inconsistent with the requirement for an eight-hour 
holding time, as pointed out by a commenter.
    In response to comments, EPA included a new entry in Table II for 
the alkylated phenols (parameters 114 to 118 in Table IC) that was 
inadvertently omitted from the proposal. Similarly, when EPA moved EPA 
Methods 1650 and 1653 to Table IC, EPA inadvertently omitted to add the 
parameters adsorbable organic halides (AOX) and chlorinated phenolics 
to Table II. The Table II information for containers, preservation, and 
holding times for these three new entries are taken from the approved 
methods.

J. Approval of Alternate Test Procedures for Limited Use at 40 CFR 
136.5

    EPA proposed changes to 40 CFR 136.4 and 136.5 that establish the 
procedures for obtaining approval for use of a nationwide or limited 
use ATP. The proposed revisions established separate sections outlining 
the procedures for obtaining EPA review and approval for nationwide use 
of an ATP (Sec. Sec.  136.4), and the procedures for obtaining approval 
for limited use of an ATP (Sec. Sec.  136.5). The proposal also 
included language to clarify that limited use approvals do not require 
the same level of supporting data that would be required for nationwide 
approvals and that limited use approvals are not intended to be used as 
a means to avoid the full examination of comparability that is required 
for an application for approval of an alternative test procedure for 
nationwide use.
    Today's rule finalizes these sections as proposed with one 
exception. EPA received comments that the proposed language under Sec.  
136.5 does not require that comparability data be submitted when 
seeking a Regional limited use ATP approval. EPA agrees that 
comparability data is an essential component of the ATP approval 
process and had inadvertently omitted this language. As a result, the 
Agency added language in today's final rule that requires an applicant 
to provide comparability data specific to the limited use for the 
performance of the proposed alternative test procedure relative to the 
performance of the reference method.

K. Revisions to Language at Sec.  136.6

    EPA proposed to revise the section on method modification 
provisions at 40 CFR 136.6 to provide more examples of allowed and 
prohibited method modifications. Acceptable reasons for an analyst to 
modify a method include analytical practices that lower detection 
limits, improve precision, reduce interferences, lower laboratory 
costs, and promote environmental stewardship by reducing generation of 
laboratory wastes. Acceptable modifications may use existing or 
emerging analytical technologies that achieve these ends provided that 
they do not depart substantially from the underlying chemical 
principles in methods currently approved in 40 CFR part 136. Analysts 
may use the examples in this section to help assess whether the 
modifications require an ATP and if not, to document that their 
modification is acceptable. The additional examples provide further 
guidance to laboratories and permittees on allowable method 
modifications that do not require an application through the ATP 
program. Proposal comments generally expressed support for allowing the 
flexibility to make certain changes to methods and for the specific 
examples of allowable changes included in the proposal. In addition, 
some commenters suggested revisions to clarify EPA's intent in Sections 
(b)(4) and (b)(5) of 40 CFR 136.6. EPA reviewed the suggestions and 
agrees with commenters that the revisions will provide additional 
clarity. In addition, as discussed in Section III.D of this preamble, 
EPA added the use of axially viewed torch as an allowable modification 
to Method 200.7. Today's rule includes the following revisions to the 
regulatory text:
    (a) Adds language to Section (b)(3) to clarify that modifications 
to sample collection, preservation, and holding time do not fall within 
the scope of 136.6,
    (b) Revises the language at (b)(4)(T) be more specific with respect 
to the use of gas diffusion across a hydrophobic semi-permeable 
membrane to separate the analyte of interest from the sample matrix in 
place of manual or automated distillation for the analysis of certain 
analytes,
    (c) Revises the equation for Relative Standard Error (RSE) in 
(b)(4)(J) to make it consistent with the description in other EPA 
methods, and
    (d) Adds the use of an axially viewed torch with Method 200.7 as an 
allowable modification.

L. Revisions to New Quality Assurance and Quality Control Language

    For today's rule, EPA added some introductory language to this 
section to clarify the new requirements. EPA added this language to 
provide some additional clarity as to when the new requirements are 
applicable and, thus, must be incorporated into the laboratory's 
documented standard operating procedures. Additional discussion of the 
revisions is provided under section IV.C below.

M. Withdrawal of Appendices at 40 CFR Part 136

    EPA proposed to incorporate by reference in Table IB all of the 
methods printed in 40 CFR part 136 Appendices A and C, and to remove 
most of the information in Appendix D. The methods in Appendix A are 
EPA Method Numbers 601 through 613, 624, 625, 1613B, 1624B, and 1625B. 
Appendix C contains EPA Method 200.7, ``Determination of Metals and 
Trace Elements in Water and Wastes by Inductively Coupled Plasma--
Atomic Emission Spectrometry''. However, Federal regulations at 1 CFR 
part 51.7(c)(1) prohibit the incorporation by reference of material 
previously published in the Federal Register. Thus, EPA is not 
withdrawing Appendices A or C. Because EPA Method 200.7 has been 
revised, EPA is replacing the current version of this method in 
Appendix C with Rev. 4.4 of Method 200.7. All of these methods are 
readily accessible from a variety of sources, including EPA's CWA 
methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm.
    The rule also removes most of the data from Appendix D for all EPA 
methods that are no longer approved, and retains only the Precision and 
Recovery Statements for EPA Method 279.2 for thallium and EPA Method 
289.2 for zinc, and corrects

[[Page 29766]]

typographical errors in the Appendix. The current version of Appendix D 
will be available online at the CWA methods Web site for historical 
purposes.

N. Revisions at 40 CFR Part 430 (Pulp, Paper, and Paperboard Point 
Source Category)

    EPA also proposed to remove Appendix A at 40 CFR part 430 and to 
incorporate by reference the methods in this Appendix. Appendix A 
contains two methods, EPA Method 1650 for adsorbable organic halides or 
AOX, and EPA Method 1653 for chlorinated phenolics. As explained above, 
we cannot incorporate by reference this material, so Appendix A remains 
unchanged in the Code of Federal Regulations. These methods are also 
readily available from a variety of sources, including EPA's CWA 
methods Web site http://water.epa.gov/scitech/methods/cwa/index.cfm. 
EPA is also adding these two methods to Table IC for general use.

O. Revisions at 40 CFR Part 435 (Oil and Gas Extraction Point Source 
Category)

    The rule makes several changes to Part 435, Oil and Gas Extraction 
Point Source Category. First, EPA is moving the methods and associated 
quality assurance requirements from 40 CFR part 435, Subpart A 
(Offshore Subcategory) to an EPA document (``Analytic Methods for the 
Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004), and 
incorporating by reference this document in the revised regulation at 
40 CFR part 435. This approach organizes the analytical methods for the 
Offshore Subcategory into one document and allows for easier access to 
the methods for this category. The following table lists the methods 
EPA moved from part 435 to the cited document, EPA-821-R-11-004.

 EPA Method Numbers for Oil and Gas Extraction Point Source Category Analytical Methods and Prior CFR References
----------------------------------------------------------------------------------------------------------------
                                                                  Date first
            Analytical/Test method              EPA Method No.    promulgated        Previous CFR references
----------------------------------------------------------------------------------------------------------------
Static Sheen Test.............................            1617            1993  Subpart A, Appendix 1.
Drilling Fluids Toxicity Test.................            1619            1993  Subpart A, Appendix 2.
Procedure for Mixing Base Fluids With                     1646            2001  Subpart A, Appendix 3.
 Sediments.
Protocol for the Determination of Degradation             1647            2001  Subpart A, Appendix 4.
 of Non-Aqueous Base Fluids in a Marine Closed
 Bottle Biodegradation Test System: Modified
 ISO 11734:1995.
Determination of Crude Oil Contamination in               1655            2001  Subpart A, Appendix 5.
 Non-Aqueous Drilling Fluids by Gas
 Chromatography/Mass Spectrometry (GC/MS).
Reverse Phase Extraction (RPE) Method for                 1670            2001  Subpart A, Appendix 6.
 Detection of Oil Contamination in Non-Aqueous
 Drilling Fluids (NAF).
Determination of the Amount of Non-Aqueous                1674            2001  Subpart A, Appendix 7.
 Drilling Fluid (NAF) Base Fluid from Drill
 Cuttings by a Retort Chamber (Derived from
 API Recommended Practice 13B-2).
----------------------------------------------------------------------------------------------------------------

    As noticed in the proposed rule, EPA is also incorporating 
additional quality assurance procedures in the marine anaerobic 
biodegradation method (Appendix 4 of Subpart A of part 435) and is 
correcting some erroneous references and omissions in the method for 
identification of crude oil contamination (Appendix 5 of Subpart A of 
part 435) into the new document (EPA-821-R-11-004).
    EPA promulgated the use of the marine anaerobic biodegradation 
method (closed bottle test, ISO 11734:1995 as clarified by Appendix 4 
to Subpart A of part 435) as an Appendix to the rule in 2001 because it 
most closely modeled the ability of a drilling fluid to biodegrade 
anaerobically in marine environments (January 22, 2001; 66 FR 6864). 
Subsequent to this promulgation, EPA incorporated additional quality 
assurance procedures for the marine anaerobic biodegradation method in 
the NPDES permit for the Western Gulf of Mexico (``Final NPDES General 
Permit for New and Existing Sources and New Dischargers in the Offshore 
Subcategory of the Oil and Gas Extraction Category for the Western 
Portion of the Outer Continental Shelf of the Gulf of Mexico,'' 
GMG290000, Appendix B). The additional quality assurance instructions 
in the GMG290000 more clearly describe the sample preparation and 
compliance determination steps. Specifically, these additional quality 
assurance procedures clarify that users must only use headspace gas to 
determine compliance with the Part 435 effluent guidelines. EPA worked 
with the same industry consortium that assisted EPA in the development 
of the analytical methods used in the effluent guidelines for the Oil 
and Gas Extraction point source category (40 CFR part 435) to develop 
these additional quality assurance measures. Thus, the quality 
assurance procedures are generally applicable to this industry.
    Additionally, as noticed in the proposed rule, EPA is correcting 
some erroneous references and omissions in the method for 
identification of crude oil contamination (Appendix 5 of Subpart A of 
Part 435), as follows:
    a. Adding a schematic flow for qualitative identification of crude 
oil, which was erroneously omitted in Appendix 5 to Subpart A of part 
435,
    b. Correcting erroneous citations in sections 9.5, 9.6, 11.3, and 
11.3.1 of Appendix 5, and
    c. Adding a missing ``<'' (less than) sign for identification of 
crude oil contamination in the asphaltene crude discussion at Section 
11.5.4.2. The asphaltene discussion now reads as follows: ``Asphaltene 
crude oils with API gravity < 20 may not produce chromatographic peaks 
strong enough to show contamination at levels of the calibration. 
Extracted ion peaks should be easier to see than increased intensities 
for the C8 to C13 peaks. If a sample of asphaltene crude from the 
formation is available, a calibration standard shall be prepared.''
    EPA received three comments on the proposed changes. One commenter 
was concerned that the EPA document (EPA-821-R-11-004) would not have 
the same legal status as publishing the methods in the CFR. EPA 
disagrees with this comment. The incorporation by reference of this 
document has the same legal standing as publishing the text of the 
methods in the CFR. EPA has a long standing practice of publishing test 
methods using incorporation by reference and the cited test methods are

[[Page 29767]]

as legally enforceable as those published in full in the CFR. EPA is 
consolidating these methods into one document to allow for easier 
access to these methods. The incorporation by reference of this 
document also allows for better formatting of the methods and 
eliminates the redundant publication of these methods each year in the 
Code of Federal Regulations. Two other commenters had some 
recommendations for additional revisions to the EPA document (EPA-821-
R-09-013). EPA has not adopted these suggestions, given the absence of 
an opportunity for the public generally to comment on them. EPA will, 
however, consider these comments and may propose additional revisions 
in a future rulemaking. As noticed in the proposed rulemaking, the 
final rule consolidates the oil and gas test methods into a single 
document and references this document in the effluent guidelines (40 
CFR part 435). Like any other changes to an EPA-approved method, any 
changes to the methods in the EPA document (EPA-821-R-11-004) will 
require a rulemaking.

IV. Summary of EPA's Response to Comments

    The Agency received comments from 117 different individuals or 
organizations on the September 23, 2010 proposal (75 FR 58024). 
Commenters represented a variety of different interests, including 
analytical laboratories, water utilities, instrument manufacturers, 
State and local governments, trade associations, and industry. A 
summary of major public comments on the proposed rule and the Agency's 
responses is presented in this section. The public docket for this rule 
includes all of the comments received and the Agency's responses.

A. Approval of Standard Methods

    EPA proposed to revise how to identify EPA-approved Part 136 
methods that are published by the Standard Methods Committee (i.e., 
Standard Methods). EPA proposed two changes. First, EPA proposed to 
change the way it identifies an EPA-approved version of a Standard 
Method in Part 136. Second, EPA proposed to identify only the most 
recently EPA-approved version of a Standard Method in Part 136. In the 
past, EPA listed multiple versions of these methods from the 18th, 
19th, 20th editions of the printed compendiums, or from the on-line 
editions published by the Standard Methods Committee, in one or more 
columns in the Part 136.3 tables. In some cases, EPA approved more than 
one version of a Standard Method for a particular analyte in Part 136. 
Approval of several versions of the same Standard Method for an analyte 
has led to inconsistencies in how laboratories conduct these analyses, 
especially in quality assurance/quality control (QA/QC) practices. For 
this reason, EPA proposed to list only the most recently EPA-approved 
version of a Standard Method (regardless of the printed or on-line 
edition) in Part 136, with few exceptions, to identify the method with 
the year of Standard Methods approval or adoption designated by the 
last four digits in the method number (e.g., Standard Method 3113B-
2004). This approach clearly identifies the version of the standard 
method approved under Part 136 and no longer ties it to a particular 
compendium printing or edition of Standard Methods. For example, the 
exact method, Standard Method 3113B-2004 appears in the 18th, 19th, and 
20th edition of Standard Methods. Because this method is the same in 
all of these editions, a laboratory may refer to any of these editions 
when using Standard Method 3113B-2004 to measure the analytes listed in 
Table IB that are approved for this method. Thus, EPA's proposed 
approach to identify Part 136 approved standard methods does not rely 
on the particular edition of a compendium but rather on the latest 
Standard Methods approved version (by indicating the year of approval).
    EPA received numerous comments concerning the proposed changes to 
specify the method with the year of publication, rather than specifying 
the editions of Standard Methods in which the method is printed, and to 
list in Part 136 only the most recent EPA-approved version of a 
Standard Method if Standard Methods has multiple versions of a method 
for a pollutant. Some commenters expressed concern about other economic 
impacts related to laboratory start-up tests, and the need for training 
and revised standard operating procedures (SOPs) associated with the 
use of the most recently approved method. In response, EPA maintains 
that the economic impacts of start-up tests or the need for revised 
SOPs are part of the necessary expenses to maintain a laboratory 
producing data of known and acceptable quality and these costs are not 
unusual. Training new staff or training current staff on new procedures 
is also a cost that any laboratory must consider as part of doing 
business.
    EPA is aware that Standard Methods and other voluntary consensus 
organizations such as ASTM and AOAC periodically revise existing 
methods and publish them on-line and/or as a compendium. In addition to 
EPA-developed methods, the Agency approves certain methods developed by 
these and other organizations as required under the National Technology 
Transfer and Advancement Act (NTTAA) and lists them in Part 136 
periodically. Often, after EPA approves a Standard Method for use in 
Part 136, Standard Methods releases or adopts a revised version of that 
method. Generally, these revised Standard Methods involve the use of 
new technologies or improvements to previously approved methods. By 
referencing the year of adoption by Standard Methods, EPA's proposed 
change in its method citations was intended to clarify which version of 
a Standard Method is approved by EPA in Part 136. The on-line site for 
Standard Methods allows electronic release of new methods and revisions 
to existing methods prior to the publication of the compendium edition. 
Currently, Standard Methods is on a 5-7 year cycle for publication of 
the compendium and is set to release its 22nd edition soon. In some 
cases, an older version of a method approved by the Standard Methods 
Committee may appear on the on-line or compendium version of Standard 
Methods. The date of adoption is on the first page of the compendium or 
on-line method.
    Commenters are correct in pointing out that, in the event that they 
elect to use an EPA-approved Standard Method for compliance purposes, 
they would be required to use the most recently EPA-approved version of 
a Standard Method. EPA is not requiring any EPA-approved Standard 
Method in today's rule. Dischargers may use any approved Part 136 
method for compliance monitoring unless the method is specified in its 
discharge permit by the permitting authority, or the method is not 
sufficiently sensitive to comply with the permit limit. Also, if the 
discharger elects to use an EPA-approved Standard Method and does not 
have the most recent EPA-approved version, EPA finds the costs would 
not be significant. The discharger/laboratory would need to purchase 
the on-line version for the individual method and would not need to 
absorb the cost of a full subscription to the on-line service. On-line 
versions of a single method generally cost $69. Relative to the costs 
that laboratories charge to run such an analysis (generally many times 
over), this cost is negligible. Therefore, EPA does not agree with 
commenters that they will have to purchase an on-line subscription to 
Standard Methods nor does it conclude that this change will

[[Page 29768]]

present a significant financial burden to laboratories.
    Another concern raised was that any changes in Standard Methods in 
the future would be automatically approved without EPA review. This 
assertion is incorrect. Any new or revised Standard Methods would be 
proposed in the Federal Register for public comment before inclusion in 
Part 136 as required under the Clean Water Act.
    Some commenters also expressed concern that this change may affect 
the approval status of existing alternate test procedures that were 
evaluated by EPA relative to older Standard Methods. With respect to 
this concern, the Agency is not withdrawing any approved ATPs. EPA's 
withdrawal of its earlier approved versions of Standard Methods is not 
intended to affect the acceptance of any vendor-developed methods based 
on older Standard Methods that EPA previously determined to be 
acceptable versions, because the changes in Standard Methods are mostly 
editorial (e.g., clarifications, increased flexibility) and not 
procedural changes.
    In making this change in today's rule, EPA also considered that 
beginning with the publication of the 20th edition of Standard Methods, 
the Standard Methods Committee included the quality control (QC) 
procedures which are similar to the QC procedures that have been 
included by EPA in methods published in Part 136 over the last two 
decades for use in compliance monitoring programs under the Clean Water 
Act and the Safe Drinking Water Act. These procedures are specified in 
Part 1000 of the Standard Methods compendium and include the 
``essential'' quality control checks that EPA has added at 40 CFR 136.7 
as part of this final rule.

B. Preservation and Holding Time Requirements for EPA Method 624

    In response to the proposed use of EPA Method 624 as a definitive 
measurement method for acrolein and acrylonitrile, EPA received 
comments on the preservation and holding time requirements for these 
two pollutants. Commenters noted that the preservation and holding time 
requirements in Part 136 Table II for these two analytes currently 
differ from the requirements for other Method 624 analytes. 
Historically, these two analytes have had different preservation and 
requirements than the analytes currently listed in EPA Method 624. The 
current requirements in Table II date to 1984 and specify that samples 
for acrolein and acrylonitrile must be preserved at a pH in the range 
of 4 to 5. This pH range is based on concerns about degradation of 
these two analytes in strongly acidic samples (e.g., pH < 2). Footnote 
10 to Table II currently states that pH adjustment is not required if 
acrolein will not be measured, but that samples for acrolein receiving 
no pH adjustment at all must be analyzed within 3 days of sampling. In 
contrast, samples to be analyzed by EPA Method 624 for purgeable 
halocarbons are not preserved by adjusting the pH, and samples to be 
analyzed for the purgeable aromatic hydrocarbons (benzene, ethylbenzene 
and toluene) are preserved at a pH of 2. Thus, in the case where a 
permittee wants to use EPA Method 624 to measure acrolein or 
acrylonitrile in addition to other analytes included in Method 624, the 
sampler has to take an additional sample, preserve the sample for 
acrolein and acrylonitrile to pH 4 to 5, and then perform separate 
analyses. Commenters stated that EPA does not have a basis for 
requiring a different preservation and holding times for these two 
analytes and submitted data that support their assertion that sample 
preservation be allowed at either a pH of 7 or a pH of 2. EPA has 
reviewed the data, but the Agency has concluded that these data are not 
sufficient or compelling to change the current preservation and holding 
time requirements for these analytes because the data are anecdotal 
rather than the result of a well-planned and properly documented 
stability study. As a result, EPA's final rule retains the current 
sample preservation and holding time requirements for acrolein and 
acrylonitrile.

C. Quality Assurance and Quality Control Requirements

    EPA proposed to specify minimal essential quality control 
requirements at Part 136.7 for use in conducting analyses to comply 
with CWA monitoring requirements. The purpose of this requirement is to 
ensure that laboratories conducting CWA compliance monitoring use 
suitable QA/QC procedures. These QA/QC procedures were included in a 
memorandum to EPA's Regional Quality Assurance Managers (May 7, 2009 
memorandum from Richard Reding) and have been posted on EPA's Web page 
since 2009. These requirements do not apply in the case of the use of 
Part 136 approved methods that contain (or reference) their own QA/QC 
procedures, or to any non-compliance analyses. Most analytical methods 
currently listed in Part 136 contain QA/QC procedures, and permittees/
laboratories using those methods are not affected by the new 
requirement. However, there are a few older methods approved for use in 
Part 136 from the 1970s that contain no QA/QC requirements. Examples of 
Part 136 methods that lack QA/QC are Method 283.2 for titanium and 
Method 289.2 for zinc, both furnace atomic absorption methods issued in 
1978. As explained previously, an additional issue identified in the 
May 7, 2009 memorandum is that approved methods from consensus 
organizations such as Standard Methods contain the QA/QC requirements 
in a different section of their methods compendium (e.g., Standard 
Methods consolidates general QA/QC requirements for all methods in Part 
1000 of their methods compendium). Thus, EPA wants to clarify that it 
expects permittees/laboratories using Part 136 approved methods 
developed by consensus organizations for reporting compliance under the 
CWA to also comply with the QA/QC requirements listed in the 
appropriate sections in that consensus organization's compendium.
    In addition to following QA/QC requirements from consensus 
organizations for Part 136 methods without QA/QC procedures, the 
analyst has the option to follow the QA/QC published in another EPA-
approved method for that parameter that contains such QA/QC.
    As discussed in Section II.I of this preamble, EPA is reiterating 
the requirement to include QA/QC in any chemical method used for CWA 
compliance purposes. For those few Part 136 methods that lack QA/QC 
requirements, EPA is adding quality control requirements at Sec.  
136.7. EPA received numerous comments on this aspect of the proposed 
rule. Although some commenters expressed support for EPA's intent to 
ensure the quality of data by adding the new QC language, many 
commenters noted problems with the specific language, including that 
many of the QC elements do not apply to common parameters (e.g., MDLs 
cannot be calculated for pH or BOD, and surrogates and internal 
standards have no counterparts in microbiological methods). Other 
commenters expressed concern that the new language was either 
duplicative or contradicted language in existing EPA-approved methods, 
or presented conflicts with various state or national accreditation 
programs. Other commenters objected to the perceived costs associated 
with this new requirement and suggested that the QC checks simply will 
not occur, regardless of the new Part 136.7 requirement. A few 
commenters suggested improvements to the proposed language, should EPA 
decide to proceed with this new section. One commenter stated that the 
section was

[[Page 29769]]

not needed, since EPA should not be approving methods at 40 CFR part 
136 that do not already contain appropriate QA/QC. EPA addresses these 
issues below.
    With respect to the issue of applicability of the QC elements, EPA 
agrees with commenters who stated that some QC elements listed in Sec.  
136.7 may not apply to common parameters (e.g., matrix spike and matrix 
spike duplicates do not apply to pH measurements). For any of the Part 
136 methods that include (or reference) appropriate QC elements for 
these parameters, these new QA/QC requirements are not applicable. As a 
result, in today's final rule, EPA has added introductory language in 
Sec.  136.7 to clarify how laboratories should comply with this new 
requirement when one or more of the twelve essential quality control 
elements is not applicable to a method. This new introductory language 
states that in cases where one or more of the twelve QC elements do not 
apply to a given method, the laboratory may provide a written rationale 
for not including those elements in their standard operating procedures 
(SOP) for that analysis. This may be something as simple as stating 
that the given QC element does not apply to that analysis or is not 
possible to perform (as the example above for pH measurements). In 
addition, the final rule states that the twelve QC elements, as 
applicable, must be included in a laboratory's SOP for conducting an 
analysis with an approved method only when there are no QA/QC 
procedures in the Part 136 method. Again, as discussed above, this QA/
QC requirement at Part 136 does not apply to approved methods 
containing (or referencing) QA/QC procedures.
    In response to the comment that the language is either duplicative 
or contradicted in existing approved methods or accreditation programs, 
EPA has added this new section to the regulations at Part 136.7 to 
address concerns that certain approved methods do not contain QA/QC 
procedures. In those cases where an approved method incorporates these 
QC procedures (as applicable to that method), the laboratory can follow 
the method as written without creating any duplication or conflict. As 
mentioned in Section IV.A of this preamble, Standard Methods 
incorporated new QC requirements starting with the 20th edition of 
Standard Methods similar to the QC requirements included in EPA methods 
for the last two decades. Thus, most Standard Methods that are also 
approved methods in Part 136 already contain QA/QC requirements, as 
applicable. Similarly, EPA does not anticipate conflicts with 
laboratory accreditation programs because these programs generally 
follow the QC requirements in the method or as otherwise specified in 
regulatory programs. The purpose of this new section is to ensure that 
analyses conducted for compliance monitoring with CWA regulatory 
programs contain appropriate QA/QC and the Agency's view is that this 
is already occurring in most laboratories (with a few exceptions as 
discussed above). This new requirement is added to clarify that 
laboratories must implement proper QA/QC, as needed, for all CWA 
compliance related analyses to provide quality data that will withstand 
regulatory and legal challenges.
    In response to the comment that this new requirement will be 
costly, proper QA/QC is essential for obtaining results of known and 
acceptable quality. In the long run, it could be much more costly to 
use data which lacks proper QC in demonstrating or enforcing discharge 
requirements. In the short run, laboratories would only incur costs 
associated with this new requirement when the method lacks QA/QC and 
when they have not included QA/QC as part of their SOPs. EPA estimates 
that this would not have a significant impact on laboratories because 
the vast majority of Part 136 methods already include or reference QA/
QC requirements. Further, most laboratories already implement the QC 
checks prescribed by the newer methods and are already documenting 
these QC checks in the laboratory SOPs. Some of the QC checks are a 
one-time or infrequent expense (e.g., demonstration of capability and 
determination of a method detection limit), while other checks are 
routine (e.g., running a method blank). Typically, laboratories include 
QC as part of the overall analysis costs, and these costs generally add 
10-20% to the analysis cost initially for an analyst demonstration of 
capability, and less (5-10%) after the initial cost for routine QC 
(e.g., running a blank with every batch of samples). For a typical 
analysis of a metal using furnace atomic absorption, at a cost of $35-
50 per sample, the QC costs would be typically 5-10% of the total 
costs, and are generally included in the laboratory pricing schedule. 
Thus, EPA expects that any costs associated with this aspect of today's 
rule will be minimal and limited to a few older methods that some 
laboratories may still elect to use rather than the many other methods 
that contain QA/QC requirements. EPA considers these QC checks to be an 
essential part of an overall approach to producing data of known 
quality and defensibility when a particular method is used to measure 
pollutants for compliance monitoring purposes. Ignoring these QC 
checks, as a commenter suggested, is inconsistent with EPA's NPDES 
permit requirements. Thus, 40 CFR 122.41(e) of EPA's NPDES permitting 
regulations provides that the permittee ``shall at all times properly 
operate and maintain all facilities and systems of treatment and 
control * * * Proper operation and maintenance also includes adequate 
laboratory controls and appropriate quality assurance procedures * * 
*.'' In most cases, these procedures are already a part of the quality 
control practices of most laboratories and will not create an 
additional burden. However, in codifying QC requirements, EPA provides 
clarification that these procedures are mandatory, as applicable, and 
not merely optional.

V. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review and Executive 
Order 13563: Improving Regulation and Regulatory Review

    This rule is not a ``significant regulatory action'' under the 
terms of Executive Order (EO) 12866 (58 FR 51735, October 4, 1993) and 
is therefore not subject to review under EO 12866 and EO 13563.

B. Paperwork Reduction Act

    This action does not impose an information collection burden under 
the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq. 
Burden is defined at 5 CFR 1320.3(b). This rule does not impose any 
information collection, reporting, or recordkeeping requirements. This 
rule merely adds new and revised versions of testing procedures, and 
sample preservation requirements.

C. Regulatory Flexibility Act

    The Regulatory Flexibility Act (RFA) generally requires an agency 
to prepare a regulatory flexibility analysis of any rule subject to 
notice and comment rulemaking requirements under the Administrative 
Procedure Act or any other statute unless the agency certifies that the 
rule will not have a significant economic impact on a substantial 
number of small entities. Small entities include small businesses, 
small organizations, and small governmental jurisdictions.
    For purposes of assessing the impacts of this rule on small 
entities for methods under the Clean Water Act, small entity

[[Page 29770]]

is defined as: (1) A small business that meets RFA default definitions 
(based on SBA size standards) found in 13 CFR 121.201; (2) a small 
governmental jurisdiction that is a government of a city, county, town, 
school district or special district with a population less than 50,000; 
and (3) a small organization that is any not-for-profit enterprise 
which is independently owned and operated and is not dominant in its 
field.
    After considering the economic impacts of today's final rule on 
small entities, I certify that this action will not have a significant 
economic impact on a substantial number of small entities. This action 
approves new and revised versions of testing procedures. Generally, 
these changes will have a positive impact on small entities by 
increasing method flexibility, thereby allowing entities to reduce 
costs by choosing more cost-effective methods. Although EPA expects 
that in some cases the analytical costs could increase slightly due to 
additional QC requirements for a few old EPA-approved methods that lack 
QA/QC, EPA has determined that most laboratories that analyze samples 
for EPA compliance monitoring have already instituted QC requirements 
as part of their laboratory practices and this rule will not have a 
significant economic impact on a substantial number of small entities.

D. Unfunded Mandates Reform Act

    This action contains no Federal mandates under the provisions of 
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), 2 U.S.C. 
1531-1538 for State, local, or tribal governments, or the private 
sector.
    EPA has determined that this final rule contains no regulatory 
requirements that might significantly or uniquely affect small 
governments. Generally, this action will have a positive impact by 
increasing method flexibility, thereby allowing method users to reduce 
costs by choosing more cost effective methods. In some cases, 
analytical costs may increase slightly due to changes in methods, but 
these increases are neither significant, nor unique to small 
governments. This rule merely approves new and revised versions of 
testing procedures, and new sample collection, preservation, and 
holding time requirements.
    Thus, today's rule is not subject to the requirements of Section 
203 of UMRA.

E. Executive Order 13132: Federalism

    This final rule does not have federalism implications. It will not 
have substantial direct effects on the States, on the relationship 
between the national government and the States, or on the distribution 
of power and responsibilities among the various levels of government, 
as specified in Executive Order 13132 (64 FR 43255, Aug. 10, 1999). 
This rule merely approves new and revised versions of testing 
procedures, and new sample collection, preservation, and holding time 
requirements. The costs to State and local governments will be minimal. 
In fact, governments may see a cost savings because the rule adds 
flexibility for laboratories and permittees to choose between 
additional approved test methods and it also provides additional 
flexibility to modify existing test methods. Thus, laboratories and 
permittees will not make as many requests for approval of alternative 
test methods or method modifications, and the rule does not preempt 
State law. Thus, Executive Order 13132 does not apply to this rule.
    In the spirit of Executive Order 13132, and consistent with EPA 
policy to promote communications between EPA and State and local 
governments, EPA specifically solicited comment on the proposed rule 
from State and local officials.

F. Executive Order 13175: Consultation and Coordination With Indian 
Tribal Governments

    This final rule does not have tribal implications, as specified in 
Executive Order 13175, (65 FR 67249, Nov. 9, 2000). It will not have 
substantial direct effects on Tribal governments, on the relationship 
between the federal government and Indian tribes, or on the 
distribution of power and responsibilities between the federal 
government and Indian tribes. This rule merely approves new and revised 
versions of testing procedures, and new sample collection, 
preservation, and holding time requirements. The costs to tribal 
governments will be minimal. In fact, tribal governments may see a cost 
savings because the rule adds flexibility for laboratories and 
permittees to choose between additional approved test methods and it 
also provides additional flexibility to modify existing test methods. 
Thus, laboratories and permittees will not make as many requests for 
approval of alternative test methods or method modifications. Thus, 
Executive Order 13175 does not apply to this rule.
    In the spirit of Executive Order 13175, and consistent with EPA 
policy to promote communications between EPA and Indian tribes, EPA 
specifically solicited comment on the proposed rule from tribal 
officials. EPA did not receive any comments from Indian tribes.

G. Executive Order 13045: Protection of Children From Environmental 
Health Risks and Safety Risks

    EPA interprets EO 13045 (62 FR 19885, April 23, 1997) as applying 
only to those regulatory actions that concern health or safety risks, 
such that the analysis required under section 5-501 of the EO has the 
potential to influence the regulation. This action is not subject to EO 
13045 because it does not establish an environmental standard intended 
to mitigate health or safety risks. This rule approves new and revised 
versions of testing procedures, and new sample collection, 
preservation, and holding time requirements.

H. Executive Order 13211: Actions That Significantly Affect Energy 
Supply, Distribution, or Use

    This action is not subject to Executive Order 13211, ``Actions 
Concerning Regulations That Significantly Affect Energy Supply, 
Distribution, or Use'' (66 FR 28355 (May 22, 2001)) because it is not a 
significant regulatory action under Executive Order 12866.

I. National Technology Transfer and Advancement Act of 1995

    Section 12(d) of the National Technology Transfer and Advancement 
Act of 1995, (NTTAA), Public Law 104-113, section 12(d) (15 U.S.C. 272 
note), directs EPA to use voluntary consensus standards in its 
regulatory activities unless to do so would be inconsistent with 
applicable law or otherwise impractical. Voluntary consensus standards 
are technical standards (e.g., material specifications, test methods, 
sampling procedures, and business practices) that are developed or 
adopted by voluntary consensus standard bodies. The NTTAA directs EPA 
to provide Congress, through the OMB, explanations when the Agency 
decides not to use available and applicable voluntary consensus 
standards.
    This final rule approves the use of technical standards developed 
by the Standard Methods Committee, and ASTM International for use in 
compliance monitoring where the Agency has determined that those 
standards meet the needs of Clean Water Act programs. EPA is not adding 
two of the proposed ASTM methods to this final rule because these 
methods have not undergone full inter-laboratory validation as 
recommended in current Agency guidance (see Section III.C of this 
preamble). All other proposed voluntary consensus standards are 
approved in today's rule.

[[Page 29771]]

J. Executive Order 12898: Federal Actions To Address Environmental 
Justice in Minority Populations and Low-Income Populations

    Executive Order (EO) 12898 (59 FR 7629 (Feb. 16, 1994)) establishes 
federal executive policy on environmental justice. Its main provision 
directs federal agencies, to the greatest extent practicable and 
permitted by law, to make environmental justice part of their mission 
by identifying and addressing, as appropriate, disproportionately high 
and adverse human health or environmental effects of their programs, 
policies, and activities on minority populations and low-income 
populations in the United States.
    This final rule provides additional compliance methods for use by 
any facility or laboratory with no disproportionate impact on minority 
or low-income populations because it merely approves new and revised 
versions of testing procedures to measure pollutants in water.

K. Congressional Review Act

    The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the 
Small Business Regulatory Enforcement Fairness Act of 1996, generally 
provides that before a rule may take effect, the agency promulgating 
the rule must submit a rule report, which includes a copy of the rule, 
to each House of the Congress and to the Comptroller General of the 
United States. EPA will submit a report containing this rule and other 
required information to the U.S. Senate, the U.S. House of 
Representatives, and the Comptroller General of the United States prior 
to publication of the rule in the Federal Register. This action is not 
a ``major rule'' as defined by 5 U.S.C. 804(2). This rule will be 
effective June 18, 2012.

List of Subjects

40 CFR Part 136

    Environmental protection, Test procedures, Incorporation by 
reference, Reporting and recordkeeping requirements, Water pollution 
control.

40 CFR Part 260

    Environmental protection, Administrative practice and procedure, 
Confidential business information, Hazardous waste, Incorporation by 
reference, Reporting and recordkeeping requirements.

40 CFR Part 423

    Environmental protection, Steam Electric Power Generating Point 
Source Category, Incorporation by reference, Reporting and 
recordkeeping requirements, Water pollution control.

40 CFR Part 430

    Environmental protection, Pulp, Paper, and Paperboard Point Source 
Category, Incorporation by reference, Reporting and recordkeeping 
requirements, Water pollution control.

40 CFR Part 435

    Environmental protection, Oil and Gas Extraction Point Source 
Category, Incorporation by reference, Reporting and recordkeeping 
requirements, Water pollution control.

    Dated: April 17, 2012.
Lisa P. Jackson,
Administrator.
    For the reasons set out in the preamble, title 40, chapter I of the 
Code of Federal Regulations, is amended as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS 
OF POLLUTANTS

0
1. The authority citation for Part 136 continues to read as follows:

    Authority:  Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 
91 Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water 
Pollution Control Act Amendments of 1972 as amended by the Clean 
Water Act of 1977.)


0
2. Section 136.1 is amended by revising paragraph (a) to read as 
follows:


Sec.  136.1  Applicability.

    (a) The procedures prescribed herein shall, except as noted in 
Sec. Sec.  136.4, 136.5, and 136.6, be used to perform the measurements 
indicated whenever the waste constituent specified is required to be 
measured for:
    (1) An application submitted to the Administrator, or to a State 
having an approved NPDES program for a permit under section 402 of the 
Clean Water Act of 1977, as amended (CWA), and/or to reports required 
to be submitted under NPDES permits or other requests for quantitative 
or qualitative effluent data under parts 122 to 125 of title 40; and
    (2) Reports required to be submitted by dischargers under the NPDES 
established by parts 124 and 125 of this chapter; and
    (3) Certifications issued by States pursuant to section 401 of the 
CWA, as amended.
* * * * *

0
3. Section 136.3 is amended:
0
a. By revising paragraph (a) introductory text and Tables IA, IB, IC, 
ID, IG, and IH;
0
b. By revising paragraph (b);
0
c. By revising paragraph (e) introductory text;
0
d. By revising Table II to paragraph (e).
    These revisions and additions read as follows:


Sec.  136.3  Identification of test procedures.

    (a) Parameters or pollutants, for which methods are approved, are 
listed together with test procedure descriptions and references in 
Tables IA, IB, IC, ID, IE, IF, IG, and IH. The methods listed in Tables 
IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see 
paragraph (b) of this section, with the exception of EPA Methods 200.7, 
601-613, 624, 625, 1613, 1624, and 1625. The full texts of Methods 601-
613, 624, 625, 1613, 1624, and 1625 are printed in appendix A of this 
part 136, and the full text of Method 200.7 is printed in appendix C of 
this part 136. The full text for determining the method detection limit 
when using the test procedures is given in appendix B of this part 136. 
The full text of Method 200.7 is printed in appendix C of this part 
136. In the event of a conflict between the reporting requirements of 
40 CFR Parts 122 and 125 and any reporting requirements associated with 
the methods listed in these tables, the provisions of 40 CFR Parts 122 
and 125 are controlling and will determine a permittee's reporting 
requirements. The full text of the referenced test procedures are 
incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and 
IH. The discharge parameter values for which reports are required must 
be determined by one of the standard analytical test procedures 
incorporated by reference and described in Tables IA, IB, IC, ID, IE, 
IF, IG, and IH or by any alternate test procedure which has been 
approved by the Administrator under the provisions of paragraph (d) of 
this section and Sec. Sec.  136.4 and 136.5. Under certain 
circumstances paragraph (c) of this section, Sec.  136.5(a) through (d) 
or 40 CFR 401.13, other additional or alternate test procedures may be 
used.

[[Page 29772]]



                                     Table IA--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units               Method \1\                EPA              Standard methods        AOAC, ASTM,  USGS              Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
    1. Coliform (fecal), number     Most Probable Number   p. 132 \3\...........  9221 C E-2006.                                    ....................
     per 100 mL or number per gram   (MPN), 5 tube, 3      1680 11,15...........
     dry weight.                     dilution, or          1681 11,20...........
                                    Membrane filter (MF)   p. 124 \3\...........  9222 D-1997..........  B-0050-85 \4\.             ....................
                                     \2\, single step
    2. Coliform (fecal) in          MPN, 5 tube, 3         p. 132 \3\...........  9221 C E-2006.                                    ....................
     presence of chlorine, number    dilution, or
     per 100 mL.
                                    MF \2\, single step    p. 124 \3\...........  9222 D-1997.                                      ....................
                                     \5\.
    3. Coliform (total), number     MPN, 5 tube, 3         p. 114 \3\...........  9221 B-2006.                                      ....................
     per 100 mL.                     dilution, or.
                                    MF \2\, single step    p. 108 \3\...........  9222 B-1997..........  B-0025-85 \4\              ....................
                                     or two step.
    4. Coliform (total), in         MPN, 5 tube, 3         p. 114 \3\...........  9221 B-2006                                       ....................
     presence of chlorine, number    dilution, or
     per 100 mL.
                                    MF \2\ with            p. 111 \3\...........  9222 (B + B.5c)-1997.                             ....................
                                     enrichment \5\.
5. E. coli, number per 100 mL \21\  MPN \6,8,16\ multiple  .....................  9221B.1-2006/9221F-                               ....................
                                     tube, or.                                     2006 12,14.
                                    multiple tube/         .....................  9223 B-200 4\13\.....  991.15 \10\..............  Colilert[supreg]13,1
                                     multiple well, or                                                                               8
                                                                                                                                    Colilert-
                                                                                                                                     18[supreg]13,17,18
                                    MF 2,6,7,8 single      1603 \22\............  .....................  .........................  mColiBlue-
                                     step.                                                                                           24[supreg]19
    6. Fecal streptococci, number   MPN, 5 tube 3          p. 139 \3\...........  9230 B-2007.                                      ....................
     per 100 mL.                     dilution, or
                                    MF \2\, or...........  p. 136 \3\...........  9230 C-2007..........  B-0055-85 \4\              ....................
                                    Plate count..........  p. 143 \3\.                                                              ....................
    7. Enterococci, number per 100  MPN 6,8, multiple      .....................  .....................  D6503-99 \9\.............  Enterolert[supreg]13
     mL \22\.                        tube/multiple well,                                                                             ,24
                                     or
                                    MF 2,6,7,8 single      1600 \25\............  9230 C-2007                                       ....................
                                     step or.
                                    Plate count..........  p. 143 \3\.                                                              ....................
    8. Salmonella, number per gram  MPN multiple tube      1682 \23\.                                                               ....................
     dry weight \11\.
Aquatic Toxicity:
    9. Toxicity, acute, fresh       Ceriodaphnia dubia     2002.0.\26\                                                              ....................
     water organisms, LC50,          acute.
     percent effluent.
                                    Daphnia puplex and     2021.0.\26\                                                              ....................
                                     Daphnia magna acute.
                                    Fathead Minnow,        2000.0.\26\                                                              ....................
                                     Pimephales promelas,
                                     and Bannerfin
                                     shiner, Cyprinella
                                     leedsi, acute.
                                    Rainbow Trout,         2019.0.\26\                                                              ....................
                                     Oncorhynchus mykiss,
                                     and brook trout,
                                     Salvelinus
                                     fontinalis, acute.
    10. Toxicity, acute, estuarine  Mysid, Mysidopsis      2007.0.\26\                                                              ....................
     and marine organisms of the     bahia, acute.
     Atlantic Ocean and Gulf of
     Mexico, LC50, percent
     effluent.

[[Page 29773]]

 
                                    Sheepshead Minnow,     2004.0 \26\                                                              ....................
                                     Cyprinodon
                                     variegatus, acute.
                                    Silverside, Menidia    2006.0 \26\                                                              ....................
                                     beryllina, Menidia
                                     menidia, and Menidia
                                     peninsulae, acute.
    11. Toxicity, chronic, fresh    Fathead minnow,        1000.0.\27\
     water organisms, NOEC or        Pimephales promelas,
     IC25, percent effluent.         larval survival and
                                     growth.
                                    Fathead minnow,        1001.0.\27\
                                     Pimephales promelas,
                                     embryo-larval
                                     survival and
                                     teratogenicity.
                                    Daphnia, Ceriodaphnia  1002.0.\27\
                                     dubia, survival and
                                     reproduction.
                                    Green alga,            1003.0.\27\
                                     Selenastrum
                                     capricornutum,
                                     growth.
    12. Toxicity, chronic,          Sheepshead minnow,     1004.0.\28\
     estuarine and marine            Cyprinodon
     organisms of the Atlantic       variegatus, larval
     Ocean and Gulf of Mexico,       survival and growth.
     NOEC or IC25, percent
     effluent.
                                    Sheepshead minnow,     1005.0.\28\
                                     Cyprinodon
                                     variegatus, embryo-
                                     larval survival and
                                     teratogenicity.
                                    Inland silverside,     1006.0.\28\
                                     Menidia beryllina,
                                     larval survival and
                                     growth.
                                    Mysid, Mysidopsis      1007.0.\28\
                                     bahia, survival,
                                     growth, and
                                     fecundity.
                                    Sea urchin, Arbacia    1008.0.\28\
                                     punctulata,
                                     fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. US EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
  organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
  results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
\11\ Recommended for enumeration of target organism in sewage sludge.
\12\ The multiple-tube fermentation test is used in 9221B.1-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.

[[Page 29774]]

 
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
  glucuronidase produced by E. coli.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.1-2006, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [mu]g/mL of MUG may be used.
\15\ Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-
  10-003. April 2010. U.S. EPA.
\16\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg], Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\17\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\18\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories, Inc.
\19\ A description of the mColiBlue24[supreg] test, is available from Hach Company.
\20\ Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
\21\ Recommended for enumeration of target organism in wastewater effluent.
\22\ Method 1603: Escherichia coli (E. coli ) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (modified
  mTEC), EPA-821-R-09-007. December 2009. U.S. EPA.
\23\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-06-014. July 2006. U.S.
  EPA.
\24\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\25\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-09-016.
  December 2009. U.S. EPA.
\26\ Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA-821-R-02-012. Fifth Edition,
  October 2002. U.S. EPA.
\27\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. EPA-821-R-02-013. Fourth Edition,
  October 2002. U.S. EPA.
\28\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. EPA-821-R-02-014. Third
  Edition, October 2002. U.S. EPA.


                                                  Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                  Methodology \58\            EPA \52\            Standard methods             ASTM             USGS/AOAC/Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L.........  Electrometric endpoint  ......................  2310 B-1997..........  D1067-06.............  I-1020-85.\2\
                                      or phenolphthalein
                                      endpoint.
2. Alkalinity, as CaCO3, mg/L......  Electrometric or        ......................  2320 B-1997..........  D1067-06.............  973.43 \3\, I-1030-
                                      Colorimetric                                                                                  85.\2\
                                      titration to pH 4.5,
                                      Manual.
                                     Automatic.............  310.2 (Rev. 1974)\1\..  .....................  .....................  I-2030-85.\2\
3. Aluminum--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 D-1999 or 3111 E- .....................  I-3051-85.\2\
                                      \36\                                            1999.
                                        AA furnace.........  ......................  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        Direct Current       ......................  .....................  D4190-08.............  See footnote.\34\
                                         Plasma (DCP) \36\.
                                        Colorimetric         ......................  3500-Al B-2001.......
                                         (Eriochrome
                                         cyanine R).
4. Ammonia (as N), mg/L............  Manual distillation     350.1, Rev. 2.0 (1993)  4500-NH3 B-1997......  .....................  973.49\3\.
                                      \6\ or gas diffusion
                                      (pH > 11), followed
                                      by any of the
                                      following:
                                        Nesslerization.....  ......................  .....................  D1426-08 (A).........  973.49\3\, I-3520-
                                                                                                                                    85.\2\
                                        Titration..........  ......................  4500-NH3 C-1997......
                                        Electrode..........  ......................  4500-NH3 D-1997 or E-  D1426-08 (B).........
                                                                                      1997.
                                        Manual phenate,      ......................  4500-NH3 F-1997......  .....................  See footnote.\60\
                                         salicylate, or
                                         other substituted
                                         phenols in
                                         Berthelot reaction
                                         based methods.
                                        Automated phenate,   350.1\30\, Rev. 2.0     4500-NH3 G-1997        .....................  I-4523-85.\2\
                                         salicylate, or       (1993).                4500-NH3 H-1997......
                                         other substituted
                                         phenols in
                                         Berthelot reaction
                                         based methods.

[[Page 29775]]

 
                                        Automated electrode  Ion Chromatography....  .....................  D6919-09.............  See footnote.\7\
5. Antimony--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration \36\.
                                        AA furnace.........  ......................  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
6. Arsenic-Total,\4\ mg/L..........  Digestion,\4\ followed  206.5 (Issued 1978)
                                      by any of the           \1\.
                                      following:
                                        AA gaseous hydride.  ......................  3114 B-2009 or.......  D2972-08 (B).........  I-3062-85.\2\
                                                                                     3114 C-2009..........
                                        AA furnace.........  ......................  3113 B-2004..........  D2972-08 (C).........  I-4063-98.\49\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                        Colorimetric (SDDC)  ......................  3500-As B-1997.......  D2972-08 (A).........  I-3060-85.\2\
7. Barium-Total,\4\ mg/L...........  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999..........  .....................  I-3084-85.\2\
                                         aspiration \36\.
                                        AA furnace.........  ......................  3113 B-2004..........  D4382-02(07).........
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  .....................  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP \36\...........  ......................  .....................  .....................  See footnote.\34\
8. Beryllium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999 or.......  D3645-08 (A).........  I-3095-85.\2\
                                         aspiration.                                 3111 E-1999..........
                                        AA furnace.........  ......................  3113 B-2004..........  D3645-08 (B).........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES............  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP................  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  See footnote \61\....
                                         (aluminon).
9. Biochemical oxygen demand         Dissolved Oxygen        ......................  5210 B-2001..........  .....................  973.44\3\, p. 17.\9\,
 (BOD5), mg/L.                        Depletion.                                                                                    I-1578-78,\8\ See
                                                                                                                                    footnote.\10,63\
10. Boron--Total,\37\ mg/L.........  Colorimetric            ......................  4500-B B -2000.......  .....................  I-3112-85.\2\
                                      (curcumin).
                                        ICP/AES............  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP................  ......................  .....................  D4190-08.............  See footnote.\34\
11. Bromide, mg/L..................  Electrode.............  ......................  .....................  D1246-05.............  I-1125-85.\2\
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000, C-2000,   D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0    D-2000.
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
12. Cadmium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:

[[Page 29776]]

 
                                        AA direct            ......................  3111 B-1999..........  D3557-02(07) (A or B)  974.27,\3\ p. 37.\9\,
                                         aspiration \36\.                            or 3111 C-1999.......                          I-3135-85 \2\ or I-
                                                                                                                                    3136-85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D3557-02(07) (D).....  I-4138-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-1472-85 \2\ or I-
                                                              \68\; 200.7, Rev. 4.4                                                 4471-97.\50\
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP\36\............  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Voltametry\11\.....  ......................  .....................  D3557-02(07) (C).....
                                        Colorimetric         ......................  3500-Cd-D-1990.......
                                         (Dithizone).
13. Calcium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........  D511-08(B)...........  I-3152-85.\2\
                                         aspiration.
                                        ICP/AES............  200.5, Rev 4.2 (2003)   3120 B-1999..........  .....................  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
                                        Titrimetric (EDTA).  ......................  3500-Ca B-1997.......  D511-08 (A)..........
                                        Ion Chromatography.  ......................  .....................  D6919-09.............
14. Carbonaceous biochemical oxygen  Dissolved Oxygen        ......................  5210 B-2001..........  .....................  See footnote.\35,63\
 demand (CBOD5), mg/L\12\.            Depletion with
                                      nitrification
                                      inhibitor.
15. Chemical oxygen demand (COD),    Titrimetric...........  410.3 (Rev. 1978)\1\..  5220 B-1997..........  D1252-06 (A).........  973.46,\3\ p. 17,\9\
 mg/L.                                                                               or C-1997............                          I-3560-85.\2\
                                     Spectrophotometric,     410.4, Rev. 2.0 (1993)  5220 D-1997..........  D1252-06 (B).........  See footnotes.\13,14\
                                      manual or automatic.                                                                          I-3561-85.\2\
16. Chloride, mg/L.................  Titrimetric: (silver    ......................  4500-Cl- B-1997......  D512-04 (B)..........  I-1183-85.\2\
                                      nitrate).
                                     (Mercuric nitrate)....  ......................  4500-Cl- C-1997......  D512-04 (A)..........  973.51,\3\ I-1184-
                                                                                                                                    85.\2\
                                     Colorimetric: manual..  ......................  .....................  .....................  I-1187-85.\2\
                                     Automated               ......................  4500-Cl- E-1997......  .....................  I-2187-85.\2\
                                      (Ferricyanide).
                                     Potentiometric          ......................  4500-Cl- D-1997......
                                      Titration.
                                     Ion Selective           ......................  .....................  D512-04 (C)..........
                                      Electrode.
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2000 or.......  D4327-03.............  993.30\3\ , I-2057-
                                                              and 300.1-1, Rev 1.0   4110 C-2000..........                          90.\51\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
17. Chlorine-Total residual, mg/L..  Amperometric direct...  ......................  4500-Cl D-2000.......  D1253-08.............
                                     Amperometric direct     ......................  4500-Cl E-2000.......
                                      (low level).
                                     Iodometric direct.....  ......................  4500-Cl B-2000.......
                                     Back titration ether    ......................  4500-Cl C-2000.......
                                      end-point\15\.
                                     DPD-FAS...............  ......................  4500-Cl F-2000.......
                                     Spectrophotometric,     ......................  4500-Cl G-2000.......
                                      DPD.
                                     Electrode.............  ......................  .....................  .....................  See footnote.\16\
17A. Chlorine-Free Available, mg/L.  Amperometric direct...  ......................  4500-Cl D-2000.......  D1253-08.............
                                     Amperometric direct     ......................  4500-Cl E-2000.......
                                      (low level).
                                     DPD-FAS...............  ......................  4500-Cl F-2000.......
                                     Spectrophotometric,     ......................  4500-Cl G-2000.......
                                      DPD.
18. Chromium VI dissolved, mg/L....  0.45-micron Filtration
                                      followed by any of
                                      the following:
                                        AA chelation-        ......................  3111 C-1999..........  .....................  I-1232-85.\2\
                                         extraction.
                                        Ion Chromatography.  218.6, Rev. 3.3 (1994)  3500-Cr C-2009.......  D5257-03.............  993.23.
                                        Colorimetric         ......................  3500-Cr B-2009.......  D1687-02(07) (A).....  I-1230-85.\2\
                                         (Diphenyl-carbazid
                                         e).
19. Chromium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:

[[Page 29777]]

 
                                        AA direct            ......................  3111 B-1999..........  D1687-02(07) (B).....  974.27,\3\ I-3236-
                                         aspiration \36\.                                                                           85.\2\
                                        AA chelation-        ......................  3111 C-1999..........
                                         extraction.
                                        AA furnace.........  ......................  3113 B-2004..........  D1687-02(07) (C).....  I-3233-93.\46\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              (2003),\68\ 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500-Cr B-2009.......
                                         (Diphenyl-carbazid
                                         e).
20. Cobalt--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or 3111 C- D3558-08 (A or B)....  p. 37,\9\ I-3239-
                                         aspiration.                                  1999.                                         85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D3558-08 (C).........  I-4243-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                        DCP................  ......................  .....................  D4190-08.............  See footnote.\34\
21. Color, platinum cobalt units or  Colorimetric (ADMI)     ......................  .....................  .....................  See footnote.\18\
 dominant wavelength, hue,
 luminance purity.
                                     (Platinum cobalt).....  ......................  2120 B-2001..........  .....................  I-1250-85.\2\
                                     Spectrophotometric....
22. Copper--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or.......  D1688-07 (A or B)....  974.27,\3\ p. 37,\9\
                                         aspiration \36\.                            3111 C-1999..........                          I-3270-85 \2\ or I-
                                                                                                                                    3271-85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D1688-07 (C).........  I-4274-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500-Cu B-1999.......
                                         (Neocuproine).
                                        (Bathocuproine)....  ......................  3500-Cu C-1999.......  .....................  See footnote.\19\
23. Cyanide--Total, mg/L...........  Automated UV digestion/ ......................  .....................  .....................  Kelada-01.\55\
                                      distillation and
                                      Colorimetry.
                                     Segmented Flow          ......................  .....................  D7511-09.............
                                      Injection, In-Line
                                      Ultraviolet
                                      Digestion, followed
                                      by gas diffusion
                                      amperometry.
                                     Manual distillation     335.4, Rev. 1.0 (1993)  4500-CN- B-1999 or C-  D2036-09(A), D7284-08  10-204-00-1-X.\56\
                                      with MgCl2, followed    \57\.                   1999.
                                      by any of the
                                      following:
                                        Flow Injection, gas  ......................  .....................  D2036-09(A) D7284-08.
                                         diffusion
                                         amperometry.
                                        Titrimetric........  ......................  4500-CN- D-1999......  D2036-09(A)..........  p. 22.\9\
                                        Spectrophotometric,  ......................  4500-CN- E-1999......  D2036-09(A)..........  I-3300-85.\2\
                                         manual.
                                        Semi-Automated \20\  335.4, Rev. 1.0 (1993)  .....................  .....................  10-204-00-1-X,\56\ I-
                                                              \57\.                                                                 4302-85.\2\
                                        Ion Chromatography.  ......................  .....................  D2036-09(A)..........

[[Page 29778]]

 
                                        Ion Selective        ......................  4500-CN- F-1999......  D2036-09(A)..........
                                         Electrode.
24. Cyanide-Available, mg/L........  Cyanide Amenable to     ......................  4500-CN- G-1999......  D2036-09(B)..........
                                      Chlorination (CATC);
                                      Manual distillation
                                      with MgCl2, followed
                                      by Titrimetric or
                                      Spectrophotometric.
                                     Flow injection and      ......................  .....................  D6888-09.............  OIA-1677-09.\44\
                                      ligand exchange,
                                      followed by gas
                                      diffusion amperometry
                                      \59\.
                                     Automated Distillation  ......................  .....................  .....................  Kelada-01.\55\
                                      and Colorimetry (no
                                      UV digestion).
24.A Cyanide-Free, mg/L............  Flow Injection,         ......................  .....................  D7237-10.............  OIA-1677-09.\44\
                                      followed by gas
                                      diffusion amperometry.
                                     Manual micro-diffusion  ......................  .....................  D4282-02.............
                                      and colorimetry.
25. Fluoride--Total, mg/L..........  Manual                  ......................  4500-F- B-1997.......
                                      distillation,\6\
                                      followed by any of
                                      the following:
                                        Electrode, manual..  ......................  4500-F- C-1997.......  D1179-04 (B).........
                                        Electrode,           ......................  .....................  .....................  I-4327-85.\2\
                                         automated.
                                        Colorimetric,        ......................  4500-F- D-1997.......  D1179-04 (A).........
                                         (SPADNS).
                                        Automated            ......................  4500-F- E-1997.......
                                         complexone.
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
26. Gold--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration.
                                        AA furnace.........  231.2 (Issued 1978)\1\  3113 B-2004..........
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
27. Hardness--Total, as CaCO3, mg/L  Automated colorimetric  130.1 (Issued 1971)\1\
                                     Titrimetric (EDTA)....  ......................  2340 C-1997..........  D1126-02(07).........  973.52B,\3\ I-1338-
                                                                                                                                    85.\2\
                                     Ca plus Mg as their     ......................  2340 B-1997..........
                                      carbonates, by
                                      inductively coupled
                                      plasma or AA direct
                                      aspiration. (See
                                      Parameters 13 and
                                      33)..
28. Hydrogen ion (pH), pH units....  Electrometric           ......................  4500-H\+\ B-2000.....  D1293-99 (A or B)....  973.41,\3\ I-1586-
                                      measurement.                                                                                  85.\2\
                                     Automated electrode...  150.2 (Dec. 1982)\1\..  .....................  .....................  See footnote,\21\ I-
                                                                                                                                    2587-85.\2\
29. Iridium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration.
                                        AA furnace.........  235.2 (Issued 1978)\1\
                                        ICP/MS.............  ......................  3125 B-2009..........
30. Iron--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or.......  D1068-05 (A or B)....  974.27,\3\ I-3381-
                                         aspiration \36\.                            3111 C-1999..........                          85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D1068-05 (C).........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\

[[Page 29779]]

 
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500-Fe-1997.........  D1068-05 (D).........  See footnote.\22\
                                         (Phenanthroline).
31. Kjeldahl Nitrogen \5\--Total,    Manual digestion \20\   ......................  4500-Norg B-1997 or C- D3590-02(06) (A).....  I-4515-91.\45\
 (as N), mg/L.                        and distillation or                             1997 and 4500-NH3 B-
                                      gas diffusion,                                  1997.
                                      followed by any of
                                      the following:
                                        Titration..........  ......................  4500-NH3 C-1997......  .....................  973.48.\3\
                                        Nesslerization.....  ......................  .....................  D1426-08 (A).........
                                        Electrode..........  ......................  4500-NH3 D-1997 or E-  D1426-08 (B).........
                                                                                      1997.
                                        Semi-automated       350.1 Rev 2.0 1993....  4500-NH3 G-1997.
                                         phenate.                                    4500-NH3 H-1997......
                                        Manual phenate,      ......................  4500-NH3 F-1997......  .....................  See footnote.\60\
                                         salicylate, or
                                         other substituted
                                         phenols in
                                         Berthelot reaction
                                         based methods.
                                    --------------------------------------------------------------------------------------------------------------------
                                                              Automated Methods for TKN that do not require manual distillation
                                    --------------------------------------------------------------------------------------------------------------------
                                     Automated phenate,      351.1 (Rev. 1978)\1\..  .....................  .....................  I-4551-78.\8\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods
                                      colorimetric (auto
                                      digestion and
                                      distillation).
                                     Semi-automated block    351.2, Rev. 2.0 (1993)  4500-Norg D-1997.....  D3590-02(06) (B).....  I-4515-91.\45\
                                      digestor colorimetric
                                      (distillation not
                                      required).
                                     Block digester,         ......................  .....................  .....................  See footnote.\39\
                                      followed by Auto
                                      distillation and
                                      Titration.
                                     Block digester,         ......................  .....................  .....................  See footnote.\40\
                                      followed by Auto
                                      distillation and
                                      Nesslerization.
                                     Block Digester,         ......................  .....................  .....................  See footnote.\41\
                                      followed by Flow
                                      injection gas
                                      diffusion
                                      (distillation not
                                      required).
32. Lead--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or.......  D3559-08 (A or B)....  974.27,\3\ I-3399-
                                         aspiration \36\.                            3111 C-1999..........                          85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D3559-08 (D).........  I-4403-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Voltametry\11\.....  ......................  .....................  D3559-08 (C).........
                                        Colorimetric         ......................  3500-Pb B-1997.......
                                         (Dithizone).
33. Magnesium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........  D511-08 (B)..........  974.27,\3\ I-3447-
                                         aspiration.                                                                                85.\2\
                                        ICP/AES............  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
                                        Gravimetric........
                                        Ion Chromatography.  ......................  .....................  D6919-09.............
34. Manganese--Total,\4\ mg/L......  Digestion \4\ followed
                                      by any of the
                                      following:

[[Page 29780]]

 
                                        AA direct            ......................  3111 B-1999..........  D858-07 (A or B).....  974.27,\3\ I-3454-
                                         aspiration \36\.                                                                           85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  D858-07 (C)..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500-Mn B-1999.......  .....................  920.203.\3\
                                         (Persulfate).
                                        (Periodate)........  ......................  .....................  .....................  See footnote.\23\
35. Mercury--Total,\4\ mg/L........  Cold vapor, Manual....  245.1, Rev. 3.0 (1994)  3112 B-2009..........  D3223-02(07).........  977.22,\3\ I-3462-
                                                                                                                                    85.\2\
                                     Cold vapor, Automated.  245.2 (Issued 1974)\1\
                                     Cold vapor atomic       245.7 Rev. 2.0          .....................  .....................  I-4464-01.\71\
                                      fluorescence            (2005)\17\.
                                      spectrometry (CVAFS).
                                     Purge and Trap CVAFS..  1631E\43\.............
36. Molybdenum--Total,\4\ mg/L.....  Digestion,\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999..........  .....................  I-3490-85.\2\
                                         aspiration.
                                        AA furnace.........  ......................  3113 B-2004..........  .....................  I-3492-96.\47\
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4471-
                                                                                                                                    97.\50\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
37. Nickel--Total,\4\ mg/L.........  Digestion \4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or.......  D1886-08 (A or B)....  I-3499-85.\2\
                                         aspiration \36\.                            3111 C-1999..........
                                        AA furnace.........  ......................  3113 B-2004..........  D1886-08 (C).........  I-4503-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES \36\.......  200.5, Rev 4.2 (2003)   3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              \68\; 200.7, Rev. 4.4
                                                              (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                        DCP \36\...........  ......................  .....................  D4190-08.............  See footnote.\34\
38. Nitrate (as N), mg/L...........  Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
                                        Ion Selective        ......................  4500-NO3- D-2000.....
                                         Electrode.
                                        Colorimetric         352.1 (Issued 1971)\1\  .....................  .....................  973.50,\3\ 419D\1,7\,
                                         (Brucine sulfate).                                                                         p. 28.\9\
                                        Nitrate-nitrite N    ......................  .....................  .....................  See footnote.\62\
                                         minus Nitrite N
                                         (See parameters 39
                                         and 40).
39. Nitrate-nitrite (as N), mg/L...  Cadmium reduction,      ......................  4500-NO3- E-2000.....  D3867-04 (B).........
                                      Manual.
                                        Cadmium reduction,   353.2, Rev. 2.0 (1993)  4500-NO3- F-2000.....  D3867-04 (A).........  I-2545-90.\51\
                                         Automated.
                                        Automated hydrazine  ......................  4500-NO3- H-2000.....
                                        Reduction/           ......................  .....................  .....................  See footnote.\62\
                                         Colorimetric.
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
40. Nitrite (as N), mg/L...........  Spectrophotometric:     ......................  4500-NO2- B-2000.....  .....................  See footnote.\25\
                                      Manual.
                                        Automated            ......................  .....................  .....................  I-4540-85\2\, See
                                         (Diazotization).                                                                           footnote.\62\

[[Page 29781]]

 
                                        Automated (*bypass   353.2, Rev. 2.0 (1993)  4500-NO3- F-2000.....  D3867-04 (A).........  I-4545-85.\2\
                                         cadmium reduction).
                                        Manual (*bypass      ......................  4500-NO3- E-2000.....  D3867-04 (B).........
                                         cadmium reduction).
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
41. Oil and grease--Total            Hexane extractable      1664 Rev. A; 1664 Rev.  5520 B-2001\38\......
 recoverable, mg/L.                   material (HEM): n-      B\42\.
                                      Hexane extraction and
                                      gravimetry.
                                        Silica gel treated   1664 Rev. A; 1664 Rev.  5520 B-2001\38\ and
                                         HEM (SGT-HEM):       B\42\.                  5520 F-2001\38\.
                                         Silica gel
                                         treatment and
                                         gravimetry.
42. Organic carbon--Total (TOC), mg/ Combustion............  ......................  5310 B-2000..........  D7573-09.............  973.47\3\, p. 14.\24\
 L.
                                        Heated persulfate    ......................  5310 C 2000..........  D4839-03.............  973.47\3,\, p.
                                         or UV persulfate                            5310 D 2000..........                          14.\24\
                                         oxidation.
43. Organic nitrogen (as N), mg/L..  Total Kjeldahl N
                                      (Parameter 31) minus
                                      ammonia N (Parameter
                                      4).
44. Ortho-phosphate (as P), mg/L...                          Ascorbic acid method:
                                        Automated..........  365.1, Rev. 2.0 (1993)  4500-P F-1999 or G-    .....................  973.56\3\, I-4601-
                                                                                      1999.                                         85.\2\
                                        Manual single        ......................  4500-P E-1999........  D515-88(A)...........  973.55.\3\
                                         reagent.
                                        Manual two reagent.  365.3 (Issued 1978)\1\
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30.\3\
                                                              and 300.1-1, Rev 1.0
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
45. Osmium--Total\4\, mg/L.........  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999..........
                                         aspiration,.
                                        AA furnace.........  252.2 (Issued 1978)\1\
46. Oxygen, dissolved, mg/L........  Winkler (Azide          ......................  4500-O B-2001, C-      D888-09 (A)..........  973.45B\3\, I-1575-
                                      modification).                                  2001, D-2001, E-                              78.\8\
                                                                                      2001, F-2001.
                                        Electrode..........  ......................  4500-O G-2001........  D888-09 (B)..........  I-1576-78.\8\
                                        Luminescence Based   ......................  .....................  D888-09 (C)..........  See footnote\63\
                                         Sensor.                                                                                   See footnote.\64\
47. Palladium--Total,\4\ mg/L......  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration.
                                        AA furnace.........  253.2\1\(Issued 1978).
                                        ICP/MS.............  ......................  3125 B-2009..........
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
48. Phenols, mg/L..................  Manual                  420.1\1\(Rev. 1978)...  5530 B-2005..........  D1783-01.............
                                      distillation\26\,
                                      followed by any of
                                      the following:
                                        Colorimetric (4AAP)  420.1\1\(Rev. 1978)...  5530 D-2005\27\......  D1783-01 (A or B)....
                                         manual.
                                        Automated            420.4 Rev. 1.0 (1993).
                                         colorimetric
                                         (4AAP).
49. Phosphorus (elemental), mg/L...  Gas-liquid              ......................  .....................  .....................  See footnote.\28\
                                      chromatography.
50. Phosphorus--Total, mg/L........  Digestion\20\,          ......................  4500-P B(5)-1999.....  .....................  973.55.\3\
                                      followed by any of
                                      the following:
                                        Manual.............  365.3\1\(Issued 1978).  4500-P E-1999........  D515-88 (A)..........
                                        Automated ascorbic   365.1 Rev. 2.0 (1993).  4500-P F-1999, G-      .....................  973.56\3\, I-4600-
                                         acid reduction.                              1999, H-1999.                                 85.\2\
                                        ICP/AES\4, 36\.....  200.7, Rev. 4.4 (1994)  3120 B-1999..........  .....................  I-4471-97.\50\

[[Page 29782]]

 
                                        Semi-automated       365.4\1\ (Issued 1974)  .....................  D515-88 (B)..........  I-4610-91.\48\
                                         block digestor
                                         (TKP digestion).
51. Platinum--Total,\4\ mg/L.......  Digestion\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration.
                                        AA furnace.........  255.2 (Issued 1978)\1\
                                        ICP/MS.............  ......................  3125 B-2009..........
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
52. Potassium--Total,\4\ mg/L......  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........  .....................  973.53\3\, I-3630-
                                         aspiration.                                                                                85.\2\
                                        ICP/AES............  200.7, Rev. 4.4 (1994)  3120 B-1999..........
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
                                        Flame photometric..  ......................  3500-K B-1997........
                                        Electrode..........  ......................  3500-K C-1997........
                                        Ion Chromatography.  ......................  .....................  D6919-09.............
53. Residue--Total, mg/L...........  Gravimetric, 103-       ......................  2540 B-1997..........  .....................  I-3750-85.\2\
                                      105[deg].
54. Residue--filterable, mg/L......  Gravimetric, 180[deg].  ......................  2540 C-1997..........  D5907-03.............  I-1750-85.\2\
55. Residue--non-filterable (TSS),   Gravimetric, 103-       ......................  2540 D-1997..........  D5907-03.............  I-3765-85.\2\
 mg/L.                                105[deg] post washing
                                      of residue.
56. Residue--settleable, mg/L......  Volumetric, (Imhoff     ......................  2540 F-1997..........
                                      cone), or gravimetric.
57. Residue--Volatile, mg/L........  Gravimetric, 550[deg].  160.4 (Issued 1971)\1\  2540-E-1997..........  .....................  I-3753-85.\2\
58. Rhodium--Total,\4\ mg/L........  Digestion\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration, or.
                                        AA furnace.........  265.2 (Issued 1978)\1\
                                        ICP/MS.............  ......................  3125 B-2009..........
59. Ruthenium--Total,\4\ mg/L......  Digestion\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration, or.
                                        AA furnace.........  267.2\1\..............
                                        ICP/MS.............  ......................  3125 B-2009..........
60. Selenium--Total,\4\ mg/L.......  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA furnace.........  ......................  3113 B-2004..........  D3859-08 (B).........  I-4668-98.\49\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES\36\........  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14\3\, I-4020-
                                                                                                                                    05.\70\
                                        AA gaseous hydride.  ......................  3114 B-2009, or 3111   D3859-08 (A).........  I-3667-85.\2\
                                                                                      C-2009.
61. Silica--Dissolved,\37\ mg/L....  0.45-micron filtration
                                      followed by any of
                                      the following:
                                        Colorimetric,        ......................  4500-SiO2 C-1997.....  D859-05..............  I-1700-85.\2\
                                         Manual.
                                        Automated            ......................  4500-SiO2 E-1997 or F- .....................  I-2700-85.\2\
                                         (Molybdosilicate).                           1997.
                                        ICP/AES............  200.5, Rev 4.2          3120 B-1999..........  .....................  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
62. Silver--Total,\4, 31\ mg/L.....  Digestion\4, 29\,
                                      followed by any of
                                      the following:
                                        AA direct            ......................  3111 B-1999 or         .....................  974.27\3\, p. 37\9\,
                                         aspiration.                                 3111 C-1999..........                          I-3720-85.\2\
                                        AA furnace.........  ......................  3113 B-2004..........  .....................  I-4724-89.\51\
                                        STGFAA.............  200.9, Rev. 2.2 (1994)

[[Page 29783]]

 
                                        ICP/AES............  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14\3\, I-4471-
                                                                                                                                    97.\50\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
63. Sodium--Total,\4\ mg/L.........  Digestion\4,\,
                                      followed by any of
                                      the following:
                                        AA direct            ......................  3111 B-1999..........  .....................  973.54\3\, I-3735-
                                         aspiration.                                                                                85.\2\
                                        ICP/AES............  200.5, Rev 4.2          3120 B-1999..........  .....................  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
                                        Flame photometric..  ......................  3500-Na B-1997.......
                                        Ion Chromatography.  ......................  .....................  D6919-09.............
64. Specific conductance, micromhos/ Wheatstone bridge.....  120.1\1\(Rev. 1982)...  2510 B-1997..........  D1125-95(99) (A).....  973.40\3\, I-2781-
 cm at 25[deg]C.                                                                                                                    85.\2\
65. Sulfate (as SO4), mg/L.........  Automated colorimetric  375.2, Rev. 2.0 (1993)  4500-SO4\2-\ F-1997
                                                                                      or G-1997.
                                        Gravimetric........  ......................  4500-SO4\2-\ C-1997    .....................  925.54.\3\
                                                                                      or D-1997.
                                        Turbidimetric......  ......................  4500-SO4\2-\ E-1997..  D516-07..............
                                        Ion Chromatography.  300.0, Rev 2.1 (1993)   4110 B-2000 or C-2000  D4327-03.............  993.30\3\, I-4020-
                                                              and 300.1-1, Rev 1.0                                                  05.\70\
                                                              (1997).
                                        CIE/UV.............  ......................  4140 B-1997..........  D6508-00(05).........  D6508, Rev. 2.\54\
66. Sulfide (as S), mg/L...........  Sample Pretreatment...  ......................  4500-S2- B, C-2000...
                                        Titrimetric          ......................  4500-S2-F-2000.......  .....................  I-3840-85.\2\
                                         (iodine).
                                        Colorimetric         ......................  4500-S2-D-2000.......
                                         (methylene blue).
                                        Ion Selective        ......................  4500-S2-G-2000.......  D4658-08.............
                                         Electrode.
67. Sulfite (as SO3), mg/L.........  Titrimetric (iodine-    ......................  4500-SO32-B-2000.....
                                      iodate).
68. Surfactants, mg/L..............  Colorimetric            ......................  5540 C-2000..........  D2330-02.............
                                      (methylene blue).
69. Temperature, [deg]C............  Thermometric..........  ......................  2550 B-2000..........  .....................  See footnote.\32\
70. Thallium-Total,\4\ mg/L........  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999..........
                                         aspiration.
                                        AA furnace.........  279.2\1\(Issued 1978).  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES............  200.7, Rev. 4.4         3120 B-1999..........  D1976-07.............
                                                              (1994); 200.5 Rev.
                                                              4.2 (2003)\68\.
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14\3\, I-4471-
                                                                                                                                    97.\50\
71. Tin-Total,\4\ mg/L.............  Digestion\4\, followed
                                      by any of the
                                      following:.
                                        AA direct            ......................  3111 B-1999..........  .....................  I-3850-78.\8\
                                         aspiration.
                                        AA furnace.........  ......................  3113 B-2004..........
                                        STGFAA.............  200.9, Rev. 2.2 (1994)
                                        ICP/AES............  200.5, Rev 4.2
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\
72. Titanium-Total,\4\ mg/L........  Digestion\4\ followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999..........
                                         aspiration.
                                        AA furnace.........  283.2\1\(Issued 1978).
                                        ICP/AES............  200.7, Rev. 4.4 (1994)
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14.\3\

[[Page 29784]]

 
                                        DCP................  ......................  .....................  .....................  See footnote.\34\
73. Turbidity, NTU\53\.............  Nephelometric.........  180.1, Rev. 2.0 (1993)  2130 B-2001..........  D1889-00.............  I-3860-85.\2\
                                                                                                                                   See footnote.\65\
                                                                                                                                   See footnote.\66\
                                                                                                                                   See footnote.\67\
74. Vanadium-Total,\4\ mg/L........  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 D-1999..........
                                         aspiration.
                                        AA furnace.........  ......................  3113 B-2004..........  D3373-03(07).........
                                        ICP/AES............  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14\3\, I-4020-
                                                                                                                                    05.\70\
                                        DCP................  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500-V B-1997........
                                         (Gallic Acid).
75. Zinc-Total\4\, mg/L............  Digestion\4\, followed
                                      by any of the
                                      following:
                                        AA direct            ......................  3111 B-1999 or 3111 C- D1691-02(07) (A or B)  974.27\3\, p. 37\9\,
                                         aspiration\36\.                              1999.                                         I-3900-85.\2\
                                        AA furnace.........  289.2\1\(Issued 1978).
                                        ICP/AES\36\........  200.5, Rev 4.2          3120 B-1999..........  D1976-07.............  I-4471-97.\50\
                                                              (2003)\68\; 200.7,
                                                              Rev. 4.4 (1994).
                                        ICP/MS.............  200.8, Rev. 5.4 (1994)  3125 B-2009..........  D5673-05.............  993.14\3\, I-4020-
                                                                                                                                    05.\70\
                                        DCP\36\............  ......................  .....................  D4190-08.............  See footnote.\34\
                                        Colorimetric         ......................  3500 Zn B-1997.......  .....................  See footnote.\33\
                                         (Zincon).
76. Acid Mine Drainage.............  ......................  1627\69\..............
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB Notes:
\1\ Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.
\2\ Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological
  Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.
\3\ Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC
  International.
\4\ For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion
  procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable
  form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in
  Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to
  gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a
  combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as
  Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA/600R-94/111, May, 1994, and is reproduced in
  EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain
  elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic
  absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced
  method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission
  spectrometry (ICP-AES), the direct current plasma (DCP) technique or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use
  EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes as indicated in Table IB);
  the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the
  digestion procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation
  step is not necessary: however, manual distillation will be required to resolve any controversies. In general, the analytical method should be
  consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to
  evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation
  step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future
  analysis. Comparable is defined as < 20% RPD for all tested matrices). Alternatively the two populations of spike recovery percentages may be compared
  using a recognized statistical test.
\7\ Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Bran & Luebbe Analyzing
  Technologies Inc.
\8\ The approved method is that cited in Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources
  Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. USGS.
\9\ American National Standard on Photographic Processing Effluents. April 2, 1975. American National Standards Institute.
\10\ In-Situ Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\11\ The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\ Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ``total BOD.'' The
  addition of the nitrification inhibitor is not a procedural option, but must be included to report the CBOD5 parameter. A discharger whose permit
  requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's
  permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
\13\ OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation.
\14\ Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company.
\15\ The back titration method will be used to resolve controversy.

[[Page 29785]]

 
\16\ Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research Incorporated. The calibration graph for the Orion
  residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium
  iodate/100 mL solution, respectively.
\17\ Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA.
\18\ National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253, December 1971.
\19\ Method 8506, Biocinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company.
\20\ When using a method with block digestion, this treatment is not required.
\21\ Industrial Method Number 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Autoanalyzer II. October 1976. Bran &
  Luebbe Analyzing Technologies.
\22\ Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company.
\23\ Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company.
\24\ Methods for Analysis of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological
  Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14. 1987. USGS.
\25\ Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company.
\26\ Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\ The colorimetric reaction must be conducted at a pH of 10.0  0.2.
\28\ Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography, Journal of Chromatography,
  47(3):421-426.
\29\ Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as
  an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble
  in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be
  diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
  approved method is satisfactory.
\30\ The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method
  specified quality control acceptance criteria are met.
\31\ For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in
  solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2
  to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent
  the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with
  reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as
  well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the
  cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.
\32\ ``Water Temperature-Influential Factors, Field Measurement and Data Presentation,'' Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 1, Chapter D1. 1975. USGS.
\33\ Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.
\34\ Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986-Revised
  1991. Thermo Jarrell Ash Corporation.
\35\ In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\36\ Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater
  Samples for Determination of Metals. April 16, 1992. CEM Corporation
\37\ When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\ Only use n-hexane (n-Hexane--85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil
  and Grease parameters--Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of
  other extraction solvents is prohibited.
\39\ Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical.
\40\ Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.
\41\ Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical.
\42\ Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable
  Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-
  821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane
  Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001.
\43\ Method 1631, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August
  2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality
  Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations.
\44\ Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.
\45\ Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Ammonium Plus
  Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS.
\46\ Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Chromium in Water by
  Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.
\47\ Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Molybdenum by
  Graphite Furnace Atomic Absorption Spectrophotometry. 1997.. USGS.
\48\ Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Total Phosphorus by
  Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS.
\49\ Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Arsenic and Selenium
  in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS.
\50\ Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Elements in Whole-
  water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS.
\51\ Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and
  Organic Constituents in Water and Fluvial Sediments. 1993.. USGS.
\52\ Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1-1, are published in U.S. EPA. May 1994. Methods for the Determination of
  Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in
  Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of
  Inorganic Ions in Drinking Water by Ion Chromatography.
\53\ Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach StablCal\TM\ or equivalent) are acceptable
  substitutes for formazin.
\54\ Method D6508, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate
  Electrolyte. December 2000. Waters Corp.

[[Page 29786]]

 
\55\ Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001.
  US EPA. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control
  (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the
  method, provided that the QC acceptance criteria are met.
\56\ QuikChem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of
  Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Lachat Instruments.
\57\ When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to
  distillation.
\58\ Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ``followed by'' analysis with a method,
  approved digestion and/or distillation are required prior to analysis.
\59\ Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-09 that contain particulate matter may be
  filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing
  available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the
  ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.
\60\ Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color
  reagent in Berthelot Reaction (``phenol-hypochlorite reaction'') colorimetric ammonium determination methods. For example when phenol is used as the
  color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively--see, Patton, C.J. and S.R. Crouch. March 1977.
  Anal. Chem. 49:464-469. These reaction parameters increase to pH > 12.6 and 665 nm when salicylate is used as the color reagent--see, Krom, M.D. April
  1980. The Analyst 105:305-316.
\61\ If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of Standard Methods may
  be used. This method has poorer precision and bias than the methods of choice.
\62\ Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.
\63\ Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5.
  Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for
  measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).
\64\ In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.
\65\ Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\66\ Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.
\67\ Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.
\68\ EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/
  600/R-06/115. Revision 4.2, October 2003. US EPA.
\69\ Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. US EPA.
\70\ Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell
  Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis,
  2006. USGS.
\71\ Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water With Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.


                                     Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
           Parameter \1\                     Method                 EPA \2,7\          Standard  methods             ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene....................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
2. Acenaphthylene..................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
3. Acrolein........................  GC....................  603.                                                                  .....................
                                     GC/MS.................  624 \4\, 1624B.                                                       .....................
4. Acrylonitrile...................  GC....................  603.                                                                  .....................
                                     GC/MS.................  624 \4\, 1624B.                                                       .....................
5. Anthracene......................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440B-2000...........  D4657-92 (98)........  .....................
6. Benzene.........................  GC....................  602...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
7. Benzidine.......................  Spectro-photometric...  ......................  .....................  .....................  See footnote \3\,
                                                                                                                                    p.1.
                                     GC/MS.................  625 \5\, 1625B........  6410 B-2000.                                  .....................
                                     HPLC..................  605.                                                                  .....................
8. Benzo(a)anthracene..............  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
9. Benzo(a)pyrene..................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
10. Benzo(b)fluoranthene...........  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
11. Benzo(g,h,i)perylene...........  GC....................  610.

[[Page 29787]]

 
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
12. Benzo(k)fluoranthene...........  GC....................  610.
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
13. Benzyl chloride................  GC....................  ......................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  ......................  .....................  .....................  See footnote \6\, p.
                                                                                                                                    S102.
14. Butyl benzyl phthalate.........  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
15. bis(2-Chloroethoxy) methane....  GC....................  611.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
16. bis(2-Chloroethyl) ether.......  GC....................  611.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
17. bis(2-Ethylhexyl) phthalate....  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
18. Bromodichloromethane...........  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
19. Bromoform......................  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
20. Bromomethane...................  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
21. 4-Bromophenyl phenyl ether.....  GC....................  611.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
22. Carbon tetrachloride...........  GC....................  601...................  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
23. 4-Chloro-3-methyl phenol.......  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000.                                  See footnote \9\, p.
                                                                                                                                    27.
24. Chlorobenzene..................  GC....................  601, 602..............  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
25. Chloroethane...................  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
26. 2-Chloroethylvinyl ether.......  GC....................  601.                                                                  .....................
                                     GC/MS.................  624, 1624B.                                                           .....................
27. Chloroform.....................  GC....................  601...................  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
28. Chloromethane..................  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
29. 2-Chloronaphthalene............  GC....................  612.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
30. 2-Chlorophenol.................  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
31. 4-Chlorophenyl phenyl ether....  GC....................  611.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
32. Chrysene.......................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
33. Dibenzo(a,h)anthracene.........  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
34. Dibromochloromethane...........  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
35. 1,2-Dichlorobenzene............  GC....................  601, 602..............  6200 C-1997.                                  .....................

[[Page 29788]]

 
                                     GC/MS.................  624, 1625B............  6200 B-1997..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
36. 1,3-Dichlorobenzene............  GC....................  601, 602..............  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1625B............  6200 B-1997..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
37. 1,4-Dichlorobenzene............  GC....................  601, 602..............  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1625B............  6200 B-1997..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
38. 3,3'-Dichlorobenzidine.........  GC/MS.................  625, 1625B............  6410 B-2000.                                  .....................
                                     HPLC..................  605.                                                                  .....................
39. Dichlorodifluoromethane........  GC....................  601.                                                                  .....................
                                     GC/MS.................  ......................  6200 C-1997.                                  .....................
40. 1,1-Dichloroethane.............  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
41. 1,2-Dichloroethane.............  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
42. 1,1-Dichloroethene.............  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
43. trans-1,2-Dichloroethene.......  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
44. 2,4-Dichlorophenol.............  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
45. 1,2-Dichloropropane............  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
46. cis-1,3-Dichloropropene........  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
47. trans-1,3-Dichloropropene......  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
48. Diethyl phthalate..............  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
49. 2,4-Dimethylphenol.............  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
50. Dimethyl phthalate.............  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
51. Di-n-butyl phthalate...........  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
52. Di-n-octyl phthalate...........  GC....................  606.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
53. 2, 4-Dinitrophenol.............  GC....................  604...................  6420 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     GC/MS.................  625, 1625B............  6410 B-2000.                                  .....................
54. 2,4-Dinitrotoluene.............  GC....................  609.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
55. 2,6-Dinitrotoluene.............  GC....................  609.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
56. Epichlorohydrin................  GC....................  ......................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  ......................  .....................  .....................  See footnote \6\, p.
                                                                                                                                    S102.
57. Ethylbenzene...................  GC....................  602...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
58. Fluoranthene...................  GC....................  610.                                           .....................  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
59. Fluorene.......................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
60. 1,2,3,4,6,7,8-Heptachloro-       GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
61. 1,2,3,4,7,8,9-Heptachloro-       GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
62. 1,2,3,4,6,7,8- Heptachloro-      GC/MS.................  1613B.                                                                .....................
 dibenzo-p-dioxin.
63. Hexachlorobenzene..............  GC....................  612.                                                                  .....................

[[Page 29789]]

 
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
64. Hexachlorobutadiene............  GC....................  612.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
65. Hexachlorocyclopentadiene......  GC....................  612.                                                                  .....................
                                     GC/MS.................  625 \5\, 1625B........  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
66. 1,2,3,4,7,8-Hexachloro-          GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
67. 1,2,3,6,7,8-Hexachloro-          GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
68. 1,2,3,7,8,9-Hexachloro-          GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
69. 2,3,4,6,7,8-Hexachloro-          GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
70. 1,2,3,4,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B.                                                                .....................
 p-dioxin.
71. 1,2,3,6,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B.                                                                .....................
 p-dioxin.
72. 1,2,3,7,8,9-Hexachloro-dibenzo-  GC/MS.................  1613B.                                                                .....................
 p-dioxin.
73. Hexachloroethane...............  GC....................  612.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
74. Indeno(1,2,3-c,d) pyrene.......  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
75. Isophorone.....................  GC....................  609.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
76. Methylene chloride.............  GC....................  601...................  6200 C-1997.           .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
77. 2-Methyl-4,6-dinitrophenol.....  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000.           .....................  See footnote \9\, p.
                                                                                                                                    27.
78. Naphthalene....................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27
                                     HPLC..................  610...................  6440 B-2000.                                  .....................
79. Nitrobenzene...................  GC....................  609.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  ......................  .....................  D4657-92 (98)........  .....................
80. 2-Nitrophenol..................  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
81. 4-Nitrophenol..................  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
82. N-Nitrosodimethylamine.........  GC....................  607.                                                                  .....................
                                     GC/MS.................  625 \5\, 1625B........  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
83. N-Nitrosodi-n-propylamine......  GC....................  607.                                                                  .....................
                                     GC/MS.................  625 \5\, 1625B........  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
84. N-Nitrosodiphenylamine.........  GC....................  607.                                                                  .....................
                                     GC/MS.................  625 \5\, 1625B........  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
85. Octachlorodibenzofuran.........  GC/MS.................  1613B.\10\                                                            .....................
86. Octachlorodibenzo-p-dioxin.....  GC/MS.................  1613B.\10\                                                            .....................
87. 2,2'-Oxybis(2-chloro-propane)    GC....................  611.                                                                  .....................
 [also known as bis(2-
 Chloroisopropyl) ether].
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
88. PCB-1016.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
89. PCB-1221.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
90. PCB-1232.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\

[[Page 29790]]

 
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
91. PCB-1242.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
92. PCB-1248.......................  GC....................  608.                                                                  .....................
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
93. PCB-1254.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
94. PCB-1260.......................  GC....................  608...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    43; See footnote.
                                                                                                                                    \8\
                                     GC/MS.................  625...................  6410 B-2000.                                  .....................
95. 1,2,3,7,8-Pentachloro-           GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
96. 2,3,4,7,8-Pentachloro-           GC/MS.................  1613B.                                                                .....................
 dibenzofuran.
97. 1,2,3,7,8,-Pentachloro-dibenzo-  GC/MS.................  1613B.                                                                .....................
 p-dioxin.
98. Pentachlorophenol..............  GC....................  604...................  6420 B-2000..........  .....................  See footnote \3\, p.
                                                                                                                                    140.
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
99. Phenanthrene...................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
100. Phenol........................  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
101. Pyrene........................  GC....................  610.                                                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2000..........  D4657-92 (98)........  .....................
102. 2,3,7,8-Tetrachloro-            GC/MS.................  1613B.\10\                                                            .....................
 dibenzofuran.
103. 2,3,7,8-Tetrachloro-dibenzo-p-  GC/MS.................  613, 625 \5a\, 1613B..                                                .....................
 dioxin.
104. 1,1,2,2-Tetrachloroethane.....  GC....................  601...................  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
105. Tetrachloroethene.............  GC....................  601...................  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
106. Toluene.......................  GC....................  602...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
107. 1,2,4-Trichlorobenzene........  GC....................  612...................  .....................  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
108. 1,1,1-Trichloroethane.........  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
109. 1,1,2-Trichloroethane.........  GC....................  601...................  6200 C-1997..........  .....................  See footnote \3\, p.
                                                                                                                                    130.
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
110. Trichloroethene...............  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
111. Trichlorofluoromethane........  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624...................  6200 B-1997.                                  .....................
112. 2,4,6-Trichlorophenol.........  GC....................  604...................  6420 B-2000.                                  .....................
                                     GC/MS.................  625, 1625B............  6410 B-2000..........  .....................  See footnote \9\, p.
                                                                                                                                    27.
113. Vinyl chloride................  GC....................  601...................  6200 C-1997.                                  .....................
                                     GC/MS.................  624, 1624B............  6200 B-1997.                                  .....................
114. Nonylphenol...................  GC/MS.................  ......................  .....................  D7065-06.              .....................
115. Bisphenol A (BPA).............  GC/MS.................  ......................  .....................  D7065-06.              .....................
116. p-tert-Octylphenol (OP).......  GC/MS.................  ......................  .....................  D7065-06.              .....................
117. Nonylphenol Monoethoxylate      GC/MS.................  ......................  .....................  D7065-06.              .....................
 (NP1EO).
118. Nonylphenol Diethoxylate        GC/MS.................  ......................  .....................  D7065-06.              .....................
 (NP2EO).
119. Adsorbable Organic Halides      Adsorption and          1650.\11\                                                             .....................
 (AOX).                               Coulometric Titration.

[[Page 29791]]

 
120. Chlorinated Phenolics.........  In Situ Acetylation     1653.\11\                                                             .....................
                                      and GC/MS.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([mu]g/L) except for Method 1613B, in which the parameters are expressed in picograms per liter
  (pg/L).
\2\ The full text of Methods 601-613, 624, 625, 1613B, 1624B, and 1625B are provided at Appendix A, Test Procedures for Analysis of Organic Pollutants,
  of this Part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at
  Appendix B, Definition and Procedure for the Determination of the Method Detection Limit, of this Part 136.
\3\ Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA.
\4\ Method 624 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate
  the ability to detect and quantify these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample
  introduction techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 should be used when analyzing samples
  for acrolein and acrylonitrile in the absence of such criteria in Method 624.
\5\ Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi-n-propylamine, and N-
  nitrosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these
  compounds.
\5a\ Method 625, screening only.
\6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard
  Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624,
  625, 1624B, and 1625B in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis
  must spike and analyze 10% (5% for Methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data
  quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical
  results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory
  compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk. Revised October 28, 1994. 3M Corporation.
\9\ Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of
  Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.
\10\ Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method
  1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and
  Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in Appendix A to 40 CFR Part 136 and at
  http://water.epa.gov/scitech/methods/cwa/index.cfm
\11\ Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997. U.S. EPA. Method 1653, Chlorinated Phenolics in
  Wastewater by In Situ Acetylation and GCMS. Revision A, 1997. U.S. EPA. The full text for both of these methods is provided at Appendix A in Part 430,
  The Pulp, Paper, and Paperboard Point Source Category.


                                              Table ID--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                        Method                 EPA \2,7,10\        Standard  methods            ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin.........................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-96    See footnote \3\, p.
                                                                                                               (02).                 7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
2. Ametryn........................  GC........................  507, 619.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \9\, O-3106-93; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S68.
                                    GC/MS.....................  525.2................  .....................  ....................  See footnote \14\, O-
                                                                                                                                     1121-91.
3. Aminocarb......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     94; See footnote
                                                                                                                                     \6\, p. S60.
                                    HPLC......................  632.                                                                ....................
4. Atraton........................  GC........................  619..................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68.
5. Atrazine.......................  GC........................  507, 619.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68; See
                                                                                                                                     footnote \9\, O-
                                                                                                                                     3106-93.
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
                                    GC/MS.....................  525.1, 525.2.........  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
6. Azinphos methyl................  GC........................  614, 622, 1657.......  .....................  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \6\, p. S51.
                                    GC-MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
7. Barban.........................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
8. [alpha]-BHC....................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \8\, 3M0222.
                                    GC/MS.....................  625 \5\..............  6410 B-2000..........  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.

[[Page 29792]]

 
9. [beta]-BHC.....................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \8\,
                                                                                                               96(02).               3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
10. [delta]-BHC...................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \8\,
                                                                                                               96(02).               3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
11. [gamma]-BHC (Lindane).........  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625 \5\..............  6410 B-2000..........  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
12. Captan........................  GC........................  617..................  6630 B-2000..........  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7.
13. Carbaryl......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     94, See footnote
                                                                                                                                     \6\, p. S60.
                                    HPLC......................  531.1, 632.                                                         ....................
                                    HPLC/MS...................  553..................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
14. Carbophenothion...............  GC........................  617..................  6630 B-2000..........  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73.
15. Chlordane.....................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
16. Chloropropham.................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
17. 2,4-D.........................  GC........................  615..................  6640 B-2001..........  ....................  See footnote \3\, p.
                                                                                                                                     115; See footnote
                                                                                                                                     \4\, O-3105 -83.
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
18. 4,4'-DDD......................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3105-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
19. 4,4'-DDE......................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000..........  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
20. 4,4'-DDT......................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
21. Demeton-O.....................  GC........................  614, 622.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \6\, p. S51.
22. Demeton-S.....................  GC........................  614, 622.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \6\, p. S51.
23. Diazinon......................  GC........................  507, 614, 622, 1657..  .....................  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S51.
                                    GC/MS.....................  525.2................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
24. Dicamba.......................  GC........................  615..................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     115.
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
25. Dichlofenthion................  GC........................  622.1................  .....................  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73.
26. Dichloran.....................  GC........................  608.2, 617...........  6630 B-2000..........  ....................  See footnote \3\, p.
                                                                                                                                     7;
27. Dicofol.......................  GC........................  617..................  .....................  ....................  See footnote \4\, O-
                                                                                                                                     3104-83.
28. Dieldrin......................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000..........  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
29. Dioxathion....................  GC........................  614.1, 1657..........  .....................  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73.
30. Disulfoton....................  GC........................  507, 614, 622, 1657..  .....................  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \6\ p. S51.
                                    GC/MS.....................  525.2................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
31. Diuron........................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  553..................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.

[[Page 29793]]

 
32. Endosulfan I..................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M022).
                                    GC/MS.....................  625 \5\..............  6410 B-2000..........  ....................  See footnote \13\, O-
                                                                                                                                     2002-01.
33. Endosulfan II.................  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \8\, 3M0222.
                                    GC/MS.....................  625 \5\..............  6410 B-2000..........  ....................   See footnote \13\,
                                                                                                                                     O-2002-01.
34. Endosulfan Sulfate............  GC........................  608, 617.............  6630 C-2000..........  ....................  See footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625..................  6410 B-2000..........  ....................  ....................
35. Endrin........................  GC........................  505, 508, 608, 617,    6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                 1656.                                         96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  525.1, 525.2, 625 \5\  6410 B-2000.                                 ....................
36. Endrin aldehyde...............  GC........................  608, 617.............  6630 C-2000..........  ....................  See footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  625.                                                                ....................
37. Ethion........................  GC........................  614, 614.1,1657......  .....................  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \13\, O-
                                                                                                                                     2002-01.
38. Fenuron.......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
39. Fenuron-TCA...................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
40. Heptachlor....................  GC........................  505, 508, 608, 617,    6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                 1656.                                         96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  525.1, 525.2, 625....  6410 B-2000.                                 ....................
41. Heptachlor epoxide............  GC........................  608, 617.............  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73; See footnote
                                                                                                                                     \8\, 3M0222.
                                    GC/MS.....................  625..................  6410 B-2000.                                 ....................
42. Isodrin.......................  GC........................  617..................  6630 B-2000 & C-2000.  ....................  See footnote \4\, O-
                                                                                                                                     3104-83; See
                                                                                                                                     footnote \6\, p.
                                                                                                                                     S73.
43. Linuron.......................  GC........................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  553..................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
44. Malathion.....................  GC........................  614, 1657............  6630 B-2000..........  ....................  See footnote \3\, p.
                                                                                                                                     25; See footnote
                                                                                                                                     \6\, p. S51.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
45. Methiocarb....................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     94; See footnote
                                                                                                                                     \6\, p. S60.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
46. Methoxychlor..................  GC........................  505, 508, 608.2, 617,  6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                 1656.                                         96(02).               7; See footnote
                                                                                                                                     \4\, O-3104 -83;
                                                                                                                                     See footnote \8\,
                                                                                                                                     3M0222.
                                    GC/MS.....................  525.1, 525.2.........  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
47. Mexacarbate...................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     94; See footnote
                                                                                                                                     \6\, p.S60.
                                    HPLC......................  632.                                                                ....................
48. Mirex.........................  GC........................  617..................  6630 B-2000 & C-2000.   D3086-90, D5812-     See footnote \3\, p.
                                                                                                               96(02).               7; See footnote
                                                                                                                                     \4\, O-3104-83.
49. Monuron.......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
50. Monuron-TCA...................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
51. Neburon.......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
52. Parathion methyl..............  GC........................  614, 622, 1657.......  6630 B-2000..........  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \3\, p.
                                                                                                                                     25.

[[Page 29794]]

 
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
53. Parathion ethyl...............  GC........................  614..................  6630 B-2000..........  ....................  See footnote \4\,
                                                                                                                                     page 27; See
                                                                                                                                     footnote \3\, p.
                                                                                                                                     25.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
54. PCNB..........................  GC........................  608.1, 617...........  6630 B-2000 & C-2000.   D3086-90, D5812-     See footnote \3\, p.
                                                                                                               96(02).               7.
55. Perthane......................  GC........................  617..................  .....................  D3086-90, D5812-      See footnote \4\, O-
                                                                                                               96(02).               3104-83.
56. Prometon......................  GC........................  507, 619.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68; See
                                                                                                                                     footnote \9\, O-
                                                                                                                                     3106-93.
                                    GC/MS.....................  525.2................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
57. Prometryn.....................  GC........................  507, 619.............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68; See
                                                                                                                                     footnote \9\,O-3106-
                                                                                                                                     93.
                                    GC/MS.....................  525.1, 525.2.........  .....................  ....................  See footnote \13\, O-
                                                                                                                                     2002-01.
58. Propazine.....................  GC........................  507, 619, 1656.......  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68; See
                                                                                                                                     footnote \9\, O-
                                                                                                                                     3106-93.
                                    GC/MS.....................  525.1, 525.2.                                                       ....................
59. Propham.......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
60. Propoxur......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     94; See footnote
                                                                                                                                     \6\, p. S60.
                                    HPLC......................  632.                                                                ....................
61. Secbumeton....................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68.
                                    GC........................  619.                                                                ....................
62. Siduron.......................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
                                    HPLC/MS...................  .....................  .....................  ....................  See footnote \12\, O-
                                                                                                                                     2060-01.
63. Simazine......................  GC........................  505, 507, 619, 1656..  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68; See
                                                                                                                                     footnote \9\, O-
                                                                                                                                     3106-93.
                                    GC/MS.....................  525.1, 525.2.........  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
64. Strobane......................  GC........................  617..................  6630 B-2000 & C-2000.  ....................  See footnote \3\, p.
                                                                                                                                     7.
65. Swep..........................  TLC.......................  .....................  .....................  ....................  See footnote \3\, p.
                                                                                                                                     104; See footnote
                                                                                                                                     \6\, p. S64.
                                    HPLC......................  632.                                                                ....................
66. 2,4,5-T.......................  GC........................  615..................  6640 B-2001..........  ....................  See footnote \3\, p.
                                                                                                                                     115; See footnote
                                                                                                                                     \4\, O-3105-83.
67. 2,4,5-TP (Silvex).............  GC........................  615..................  6640 B-2001..........  ....................  See footnote \3\, p.
                                                                                                                                     115; See footnote
                                                                                                                                     \4\, O-3105-83.
68. Terbuthylazine................  GC........................  619, 1656............  .....................  ....................  See footnote \3\, p.
                                                                                                                                     83; See footnote
                                                                                                                                     \6\, p. S68.
                                    GC/MS.....................  .....................  .....................  ....................  See footnote \13\, O-
                                                                                                                                     2002-01.
69. Toxaphene.....................  GC........................  505, 508, 608, 617,    6630 B-2000 & C-2000.  D3086-90, D5812-      See footnote \3\, p.
                                                                 1656.                                         96(02).               7; See footnote
                                                                                                                                     \8\; See footnote
                                                                                                                                     \4\, O-3105-83.
                                    GC/MS.....................  525.1, 525.2, 625....  6410 B-2000.                                 ....................
70. Trifluralin...................  GC........................  508, 617, 627, 1656..  6630 B-2000..........  ....................  See footnote \3\, p.
                                                                                                                                     7; See footnote
                                                                                                                                     \9\, O-3106-93.
                                    GC/MS.....................  525.2................  .....................  ....................  See footnote \11\, O-
                                                                                                                                     1126-95.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where
  entries are listed by chemical name.
\2\ The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B,
  Definition and Procedure for the Determination of the Method Detection Limit, of this Part 136.
\3\ Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA
  publication includes thin-layer chromatography (TLC) methods.
\4\ Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 5, Chapter A3. 1987. USGS.
\5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
  Method 608 is the preferred method.
\6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard
  Methods for the Examination of Water and Wastewater. 1981. American Public Health Association (APHA).

[[Page 29795]]

 
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625
  in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and
  analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in
  accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for
  that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These
  quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ Organochlorine Pesticides and PCBs in Wastewater Using Empore \TM\ Disk. Revised October 28, 1994. 3M Corporation.
\9\ Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of
  Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography With Nitrogen Phosphorus Detectors. 1994. USGS.
\10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional
  Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. The full text of Methods 608 and 625 are provided at
  Appendix A, Test Procedures for Analysis of Organic Pollutants, of this Part 136. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for
  the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA Method 525.2
  is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry,
  Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods For The Determination of Nonconventional Pesticides In Municipal and Industrial
  Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA.
\11\ Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995.
  USGS.
\12\ Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass
  Spectrometry. 2001. USGS.
\13\ Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass
  spectrometry. 2001. USGS.
\14\ Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion
  monitoring. 1992. USGS.

* * * * *

                    Table IG--Test Methods for Pesticide Active Ingredients (40 CFR Part 455)
----------------------------------------------------------------------------------------------------------------
       EPA survey code                 Pesticide name               CAS No.     EPA analytical method No.(s) \3\
----------------------------------------------------------------------------------------------------------------
8...........................  Triadimefon.....................      43121-43-3  507/633/525.1/525.2/1656
12..........................  Dichlorvos......................         62-73-7  1657/507/622/525.1/525.2
16..........................  2,4-D; 2,4-D Salts and Esters            94-75-7  1658/515.1/615/515.2/555
                               [2,4-Dichloro-phenoxyacetic
                               acid].
17..........................  2,4-DB; 2,4-DB Salts and Esters          94-82-6  1658/515.1/615/515.2/555
                               [2,4-Dichlorophenoxybutyric
                               acid].
22..........................  Mevinphos.......................       7786-34-7  1657/507/622/525.1/525.2
25..........................  Cyanazine.......................      21725-46-2  629/507
26..........................  Propachlor......................       1918-16-7  1656/508/608.1/525.1/525.2
27..........................  MCPA; MCPA Salts and Esters [2-          94-74-6  1658/615/555
                               Methyl-4-chlorophenoxyacetic
                               acid].
30..........................  Dichlorprop; Dichlorprop Salts          120-36-5  1658/515.1/615/515.2/555
                               and Esters [2-(2,4-
                               Dichlorophenoxy) propionic
                               acid].
31..........................  MCPP; MCPP Salts and Esters [2-          93-65-2  1658/615/555
                               (2-Methyl-4-chlorophenoxy)
                               propionic acid].
35..........................  TCMTB [2-(Thiocyanomethylthio)        21564-17-0  637
                               benzo-thiazole].
39..........................  Pronamide.......................      23950-58-5  525.1/525.2/507/633.1
41..........................  Propanil........................        709-98-8  632.1/1656
45..........................  Metribuzin......................      21087-64-9  507/633/525.1/525.2/1656
52..........................  Acephate........................      30560-19-1  1656/1657
53..........................  Acifluorfen.....................      50594-66-6  515.1/515.2/555
54..........................  Alachlor........................      15972-60-8  505/507/645/525.1/525.2/1656
55..........................  Aldicarb........................        116-06-3  531.1
58..........................  Ametryn.........................        834-12-8  507/619/525.2
60..........................  Atrazine........................       1912-24-9  505/507/619/525.1/525.2/1656
62..........................  Benomyl.........................      17804-35-2  631
68..........................  Bromacil; Bromacil Salts and            314-40-9  507/633/525.1/525.2/1656
                               Esters.
69..........................  Bromoxynil......................       1689-84-5  1625/1661
69..........................  Bromoxynil octanoate............       1689-99-2  1656
70..........................  Butachlor.......................      23184-66-9  507/645/525.1/525.2/1656
73..........................  Captafol........................       2425-06-1  1656
75..........................  Carbaryl [Sevin]................         63-25-2  531.1/632/553
76..........................  Carbofuran......................       1563-66-2  531.1/632
80..........................  Chloroneb.......................       2675-77-6  1656/508/608.1/525.1/525.2
82..........................  Chlorothalonil..................       1897-45-6  508/608.2/525.1/525.2/1656
84..........................  Stirofos........................        961-11-5  1657/507/622/525.1/525.2
86..........................  Chlorpyrifos....................       2921-88-2  1657/508/622
90..........................  Fenvalerate.....................      51630-58-1  1660
103.........................  Diazinon........................        333-41-5  1657/507/614/622/525.2
107.........................  Parathion methyl................        298-00-0  1657/614/622
110.........................  DCPA [Dimethyl 2,3,5,6-                1861-32-1  508/608.2/525.1/525.2/515.1 \2\/
                               tetrachloro-terephthalate].                       515.2 \2\/1656

[[Page 29796]]

 
112.........................  Dinoseb.........................         88-85-7  1658/515.1/615/515.2/555
113.........................  Dioxathion......................         78-34-2  1657/614.1
118.........................  Nabonate [Disodium cyanodithio-         138-93-2  630.1
                               imidocarbonate].
119.........................  Diuron..........................        330-54-1  632/553
123.........................  Endothall.......................        145-73-3  548/548.1
124.........................  Endrin..........................         72-20-8  1656/505/508/608/617/525.1/525.2
125.........................  Ethalfluralin...................      55283-68-6  1656/627 See footnote 1
126.........................  Ethion..........................        563-12-2  1657/614/614.1
127.........................  Ethoprop........................      13194-48-4  1657/507/622/525.1/525.2
132.........................  Fenarimol.......................      60168-88-9  507/633.1/525.1/525.2/1656
133.........................  Fenthion........................         55-38-9  1657/622
138.........................  Glyphosate [N-(Phosphonomethyl)        1071-83-6  547
                               glycine].
140.........................  Heptachlor......................         76-44-8  1656/505/508/608/617/525.1/525.2
144.........................  Isopropalin.....................      33820-53-0  1656/627
148.........................  Linuron.........................        330-55-2  553/632
150.........................  Malathion.......................        121-75-5  1657/614
154.........................  Methamidophos...................      10265-92-6  1657
156.........................  Methomyl........................      16752-77-5  531.1/632
158.........................  Methoxychlor....................         72-43-5  1656/505/508/608.2/617/525.1/
                                                                                 525.2
172.........................  Nabam...........................        142-59-6  630/630.1
173.........................  Naled...........................        300-76-5  1657/622
175.........................  Norflurazon.....................      27314-13-2  507/645/525.1/525.2/1656
178.........................  Benfluralin.....................       1861-40-1  1656/627 See footnote 1
182.........................  Fensulfothion...................        115-90-2  1657/622
183.........................  Disulfoton......................        298-04-4  1657/507/614/622/525.2
185.........................  Phosmet.........................        732-11-6  1657/622.1
186.........................  Azinphos Methyl.................         86-50-0  1657/614/622
192.........................  Organo-tin pesticides...........      12379-54-3  Ind-01/200.7/200.9
197.........................  Bolstar.........................      35400-43-2  1657/622
203.........................  Parathion.......................         56-38-2  1657/614
204.........................  Pendimethalin...................      40487-42-1  1656
205.........................  Pentachloronitrobenzene.........         82-68-8  1656/608.1/617
206.........................  Pentachlorophenol...............         87-86-5  625/1625/515.2/555/515.1/525.1/
                                                                                 525.2
208.........................  Permethrin......................      52645-53-1  608.2/508/525.1/525.2/1656/1660
212.........................  Phorate.........................        298-02-2  1657/622
218.........................  Busan 85 [Potassium                     128-03-0  630/630.1
                               dimethyldithiocarbamate].
219.........................  Busan 40 [Potassium N-                51026-28-9  630/630.1
                               hydroxymethyl-N-
                               methyldithiocarbamate].
220.........................  KN Methyl [Potassium N-methyl-          137-41-7  630/630.1
                               dithiocarbamate].
223.........................  Prometon........................       1610-18-0  507/619/525.2
224.........................  Prometryn.......................       7287-19-6  507/619/525.1/525.2
226.........................  Propazine.......................        139-40-2  507/619/525.1/525.2/1656
230.........................  Pyrethrin I.....................        121-21-1  1660
232.........................  Pyrethrin II....................        121-29-9  1660
236.........................  DEF [S,S,S-Tributyl                      78-48-8  1657
                               phosphorotrithioate].
239.........................  Simazine........................        122-34-9  505/507/619/525.1/525.2/1656
241.........................  Carbam-S [Sodium dimethyldithio-        128-04-1  630/630.1
                               carbamate].
243.........................  Vapam [Sodium                           137-42-8  630/630.1
                               methyldithiocarbamate].
252.........................  Tebuthiuron.....................      34014-18-1  507/525.1/525.2
254.........................  Terbacil........................       5902-51-2  507/633/525.1/525.2/1656
255.........................  Terbufos........................      13071-79-9  1657/507/614.1/525.1/525.2
256.........................  Terbuthylazine..................       5915-41-3  619/1656
257.........................  Terbutryn.......................        886-50-0  507/619/525.1/525.2
259.........................  Dazomet.........................        533-74-4  630/630.1/1659
262.........................  Toxaphene.......................       8001-35-2  1656/505/508/608/617/525.1/525.2
263.........................  Merphos [Tributyl                       150-50-5  1657/507/525.1/525.2/622
                               phosphorotrithioate].
264.........................  Trifluralin \1\.................       1582-09-8  1656/508/617/627/525.2
268.........................  Ziram [Zinc                             137-30-4  630/630.1
                               dimethyldithiocarbamate].
----------------------------------------------------------------------------------------------------------------
Table 1G notes:
\1\ Monitor and report as total Trifluralin.
\2\ Applicable to the analysis of DCPA degradates.
\3\ EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are available in Methods For The Determination
  of Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, Revision I,
  August 1993, U.S. EPA. EPA Methods 200.9 and 505 through 555 are available in Methods For The Determination of
  Nonconventional Pesticides In Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, August 1993,
  U.S. EPA. The full text of Methods 608, 625 and 1625 are provided at Appendix A of this Part 136. The full
  text of Method 200.7 is provided at Appendix C of this Part 136.


[[Page 29797]]


                                          Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
       Parameter and units              Method \1\               EPA            Standard methods     AOAC, ASTM, USGS                 Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
    1. Coliform (fecal), number    Most Probable Number  p. 132 \3\.........  9221 C E-2006.                            ................................
     per 100 mL or number per       (MPN), 5 tube, 3
     gram dry weight.               dilution, or.
                                   Membrane filter (MF)  p. 124 \3\.........  9222 D-1997          B-0050-85 \4\        ................................
                                    \2\, single step.
    2. Coliform (fecal) in         MPN, 5 tube, 3        p. 132 \3\.........  9221 C E-2006.                            ................................
     presence of chlorine, number   dilution, or.
     per 100 mL.
                                   MF \2\, single step   p. 124 \3\.........  9222 D-1997.                              ................................
                                    \5\.
    3. Coliform (total), number    MPN, 5 tube, 3        p. 114 \3\.........  9221 B-2006.                              ................................
     per 100 mL.                    dilution, or.
                                   MF \2\, single step   p. 108 \3\.........  9222 B-1997........  B-0025-85 \4\        ................................
                                    or two step.
    4. Coliform (total), in        MPN, 5 tube, 3        p. 114 \3\.........  9221 B-2006.                              ................................
     presence of chlorine, number   dilution, or.
     per 100 mL.
                                   MF \2\ with           p. 111 \3\.........  9222 (B+B.5c)-1997.                       ................................
                                    enrichment.
    5. E. coli, number per 100 mL  MPN 6,8,14, multiple  ...................  9221 B.1-2006/9221                        ................................
                                    tube, or.                                  F-2006 11,13.
                                   Multiple tube/        ...................  9223 B-2004 \12\...  991.15 \10\........  Colilert[supreg]12,16, Colilert-
                                    multiple well, or.                                                                   18[supreg]12,15,16.
                                   MF 2,5,6,7,8, two     1103.1 \19\........  9222 B-1997/9222 G-  D5392-93 \9\.        ................................
                                    step, or.                                  1997 \18\, 9213 D-
                                                                               2007.
                                   Single step.........  1603 \20\, 1604      ...................  ...................  mColiBlue-24[supreg]\17\.
                                                          \21\.
    6. Fecal streptococci, number  MPN, 5 tube, 3        p. 139 \3\.........  9230 B-2007.                              ................................
     per 100 mL.                    dilution, or.
                                   MF \2\, or..........  p. 136 \3\.........  9230 C-2007........  B-0055-85 \4\.       ................................
                                   Plate count.........  p. 143 \3\.........
    7. Enterococci, number per     MPN 6,8, multiple     ...................  ...................  D6503-99 \9\.......  Enterolert[supreg]12,22.
     100 mL.                        tube/multiple well,
                                    or.
                                   MF 2,5,6,7,8 two      1106.1 \23\........  9230 C-2007........  D5259-92 \9\.        ................................
                                    step, or.
                                   Single step, or.....  1600 \24\..........  9230 C-2007.                              ................................
                                   Plate count.........  p. 143 \3\.                                                    ................................
Protozoa:
    8. Cryptosporidium...........  Filtration/IMS/FA...  1622 \25\, 1623                                                ................................
                                                          \26\.
    9. Giardia...................  Filtration/IMS/FA...  1623 \26\                                                      ................................
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1H notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[micro]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
  extractables which could interfere with their growth.
\3\ Microbiological Methods for Monitoring the Environment, Water, and Wastes. EPA/600/8-78/017. 1978. US EPA.
\4\ U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of
  Aquatic Biological and Microbiological Samples. 1989. USGS.
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
  resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
  to account for the quality, character, consistency, and anticipated organism density of the water sample.
\7\ When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may
  contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
  comparability of results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
  year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
  alternate test procedure (ATP) guidelines.
\9\ Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.
\10\ Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.
\11\ The multiple-tube fermentation test is used in 9221B.1-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25
  parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-
  positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase
  on 10 percent of all total coliform-positive tubes on a seasonal basis.
\12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
  glucuronidase produced by E. coli.
\13\ After prior enrichment in a presumptive medium for total coliform using 9221B.1-2006, all presumptive tubes or bottles showing any amount of gas,
  growth or acidity within 48 h  3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.

[[Page 29798]]

 
\14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
  dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C, rather than the 24 h required for the Colilert[supreg] test, and is recommended for marine water samples.
\16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories Inc.
\17\ A description of the mColiBlue24[supreg] test may be obtained from Hach Company.
\18\ Subject total coliform positive samples determined by 9222B-1997 or other membrane filter procedure to 9222G-1997 using NA-MUG media.
\19\ Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), EPA-821-R-10-
  002. March 2010. US EPA.
\20\ Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified
  mTEC), EPA-821-R-09-007. December 2009. US EPA.
\21\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. New Medium for the
  Simultaneous Detection of Total Coliform and Escherichia coli in Water. Appl. Environ. Microbiol. 59:3534-3544 and in Method 1604: Total Coliforms and
  Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium), EPA 821-R-02-024, September 2002,
  US EPA.
\22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\23\ Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), EPA-821-R-09-015. December 2009.
  US EPA.
\24\ Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), EPA-821-R-09-016.
  December 2009. US EPA.
\25\ Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
  concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
  Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. US EPA.
\26\ Method 1623 uses a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
  determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
  of Cryptosporidium and Giardia oocysts and cysts. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002. December
  2005. US EPA.

    (b) The documents required in this section are incorporated by 
reference into this section with approval of the Director of the 
Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. 
Copies of the documents may be obtained from the sources listed in 
paragraph (b) of this section. Documents may be inspected at EPA's 
Water Docket, EPA West, 1301 Constitution Avenue NW., Room B102, 
Washington, DC (Telephone: 202-566-2426); or at the National Archives 
and Records Administration (NARA). For information on the availability 
of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. These test procedures are incorporated as they exist on 
the day of approval and a notice of any change in these test procedures 
will be published in the Federal Register. The full texts of the 
methods from the following references which are cited in Tables IA, IB, 
IC, ID, IE, IF, IG and IH are incorporated by reference into this 
regulation and may be obtained from the source identified. All costs 
cited are subject to change and must be verified from the indicated 
source.
    (1) Environmental Monitoring and Support Laboratory, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm or from: National 
Technical Information Service, 5285 Port Royal Road, Springfield, 
Virginia 22161
    (i) Microbiological Methods for Monitoring the Environment, Water, 
and Wastes. 1978. EPA/600/8-78/017, Pub. No. PB-290329/A.S.
    (A) Part III Analytical Methodology, Section B Total Coliform 
Methods, page 108. Table IA, Note 3; Table IH, Note 3.
    (B) Part III Analytical Methodology, Section B Total Coliform 
Methods, 2.6.2 Two-Step Enrichment Procedure, page 111. Table IA, Note 
3; Table IH, Note 3.
    (C) Part III Analytical Methodology, Section B Total Coliform 
Methods, 4 Most Probable Number (MPN) Method, page 114. Table IA, Note 
3; Table IH, Note 3.
    (D) Part III Analytical Methodology, Section C Fecal Coliform 
Methods, 2 Direct Membrane Filter (MF) Method, page 124. Table IA, Note 
3; Table IH, Note 3.
    (E) Part III, Analytical Methodology, Section C Fecal Coliform 
Methods, 5 Most Probable Number (MPN) Method, page 132. Table IA, Note 
3; Table IH, Note 3.
    (F) Part III Analytical Methodology, Section D Fecal Streptococci, 
2 Membrane Filter (MF) Method, page 136. Table IA, Note 3; Table IH, 
Note 3.
    (G) Part III Analytical Methodology, Section D Fecal Streptococci, 
4 Most Probable Number Method, page 139. Table IA, Note 3; Table IH, 
Note 3.
    (H) Part III Analytical Methodology, Section D Fecal Streptococci, 
5 Pour Plate Method, page 143. Table IA, Note 3; Table IH, Note 3.
    (ii) [Reserved]
    (2) Environmental Monitoring and Support Laboratory, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) Method 300.1 (including Errata Cover Sheet, April 27, 1999), 
Determination of Inorganic Ions in Drinking Water by Ion 
Chromatography, Revision 1.0, 1997. Table IB, Note 52.
    (ii) Method 551, Determination of Chlorination Disinfection 
Byproducts and Chlorinated Solvents in Drinking Water by Liquid-Liquid 
Extraction and Gas Chromatography With Electron-Capture Detection. 
1990. Table IF.
    (3) National Exposure Risk Laboratory-Cincinnati, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available from 
http://water.epa.gov/scitech/methods/cwa/index.cfm or from the National 
Technical Information Service (NTIS), 5285 Port Royal Road, 
Springfield, VA 22161. Telephone: 800-553-6847.
    (i) Methods for the Determination of Inorganic Substances in 
Environmental Samples. August 1993. EPA/600/R-93/100, Pub. No. PB 
94120821. Table IB, Note 52.
    (A) Method 180.1, Determination of Turbidity by Nephelometry. 
Revision 2.0. Table IB, Note 52.
    (B) Method 300.0, Determination of Inorganic Anions by Ion 
Chromatography. Revision 2.1. Table IB, Note 52.
    (C) Method 335.4, Determination of Total Cyanide by Semi-Automated 
Colorimetry. Revision 1.0. Table IB, Notes 52 and 57.
    (D) Method 350.1, Determination of Ammonium Nitrogen by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Notes 30 and 52.
    (E) Method 351.2, Determination of Total Kjeldahl Nitrogen by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Note 52.
    (F) Method 353.2, Determination of Nitrate-Nitrite Automated 
Colorimetry. Revision 2.0. Table IB, Note 52.

[[Page 29799]]

    (G) Method 365.1, Determination of Phosphorus by Automated 
Colorimetry. Revision 2.0. Table IB, Note 52.
    (H) Method 375.2, Determination of Sulfate by Automated 
Colorimetry. Revision 2.0. Table IB, Note 52.
    (I) Method 410.4, Determination of Chemical Oxygen Demand by Semi-
Automated Colorimetry. Revision 2.0. Table IB, Note 52.
    (ii) Methods for the Determination of Metals in Environmental 
Samples, Supplement I. May 1994. EPA/600/R-94/111, Pub. No. PB 
95125472. Table IB, Note 52.
    (A) Method 200.7, Determination of Metals and Trace Elements in 
Water and Wastes by Inductively Coupled Plasma-Atomic Emission 
Spectrometry. Revision 4.4. Table IB, Note 52.
    (B) Method 200.8, Determination of Trace Elements in Water and 
Wastes by Inductively Coupled Plasma Mass Spectrometry. Revision 5.3. 
Table IB, Note 52.
    (C) Method 200.9, Determination of Trace Elements by Stabilized 
Temperature Graphite Furnace Atomic Absorption Spectrometry. Revision 
2.2. Table IB, Note 52.
    (D) Method 218.6, Determination of Dissolved Hexavalent Chromium in 
Drinking Water, Groundwater, and Industrial Wastewater Effluents by Ion 
Chromatography. Revision 3.3. Table IB, Note 52.
    (E) Method 245.1, Determination of Mercury in Water by Cold Vapor 
Atomic Absorption Spectrometry. Revision 3.0. Table IB, Note 52.
    (4) National Exposure Risk Laboratory-Cincinnati, U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) EPA Method 200.5, Determination of Trace Elements in Drinking 
Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission 
Spectrometry. Revision 4.2, October 2003. EPA/600/R-06/115. Table IB, 
Note 68.
    (ii) EPA Method 525.2, Determination of Organic Compounds in 
Drinking Water by Liquid-Solid Extraction and Capillary Column Gas 
Chromatography/Mass Spectrometry. Revision 2.0, 1995. Table ID, Note 
10.
    (5) Office of Research and Development, Cincinnati OH. U.S. 
Environmental Protection Agency, Cincinnati OH (US EPA). Available at 
http://water.epa.gov/scitech/methods/cwa/index.cfm or from ORD 
Publications, CERI, U.S. Environmental Protection Agency, Cincinnati OH 
45268.
    (i) Methods for Benzidine, Chlorinated Organic Compounds, 
Pentachlorophenol, and Pesticides in Water and Wastewater. 1978. Table 
IC, Note 3; Table ID, Note 3.
    (ii) Methods for Chemical Analysis of Water and Wastes. March 1979. 
EPA-600/4-79-020. Table IB, Note 1.
    (iii) Methods for Chemical Analysis of Water and Wastes. Revised 
March 1983. EPA-600/4-79-020. Table IB, Note 1.
    (A) Method 120.1, Conductance, Specific Conductance, [mu]mhos at 25 
[deg]C. Revision 1982. Table IB, Note 1.
    (B) Method 130.1, Hardness, Total (mg/L as CaCO3), 
Colorimetric, Automated EDTA. Issued 1971. Table IB, Note 1.
    (C) Method 150.2, pH, Continuous Monitoring (Electrometric). 
December 1982. Table IB, Note 1.
    (D) Method 160.4, Residue, Volatile, Gravimetric, Ignition at 550 
[deg]C. Issued 1971. Table IB, Note 1.
    (E) Method 206.5, Arsenic, Sample Digestion Prior to Total Arsenic 
Analysis by Silver Diethyldithiocarbamate or Hydride Procedures. Issued 
1978. Table IB, Note 1.
    (F) Method 231.2, Gold, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (G) Method 245.2, Mercury, Automated Cold Vapor Technique. Issued 
1974. Table IB, Note 1.
    (H) Method 252.2, Osmium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (I) Method 253.2, Palladium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (J) Method 255.2, Platinum, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (K) Method 265.2, Rhodium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (L) Method 279.2, Thallium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (M) Method 283.2, Titanium, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (N) Method 289.2, Zinc, Atomic Absorption, Furnace Technique. 
Issued 1978. Table IB, Note 1.
    (O) Method 310.2, Alkalinity, Colorimetric, Automated, Methyl 
Orange. Revision 1974. Table IB, Note 1.
    (P) Method 351.1, Nitrogen, Kjeldahl, Total, Colorimetric, 
Automated Phenate. Revision 1978. Table IB, Note 1.
    (Q) Method 352.1, Nitrogen, Nitrate, Colorimetric, Brucine. Issued 
1971. Table IB, Note 1.
    (R) Method 365.3, Phosphorus, All Forms, Colorimetric, Ascorbic 
Acid, Two Reagent. Issued 1978. Table IB, Note 1.
    (S) Method 365.4, Phosphorus, Total, Colorimetric, Automated, Block 
Digestor AA II. Issued 1974. Table IB, Note 1.
    (T) Method 410.3, Chemical Oxygen Demand, Titrimetric, High Level 
for Saline Waters. Revision 1978. Table IB, Note 1.
    (U) Method 420.1, Phenolics, Total Recoverable, Spectrophotometric, 
Manual 4-AAP With Distillation. Revision 1978. Table IB, Note 1.
    (iv) Prescribed Procedures for Measurement of Radioactivity in 
Drinking Water. 1980. EPA-600/4-80-032. Table IE.
    (A) Method 900.0, Gross Alpha and Gross Beta Radioactivity. Table 
IE.
    (B) Method 903.0, Alpha-Emitting iRadio Isotopes. Table IE.
    (C) Method 903.1, Radium-226, Radon Emanation Technique. Table IE.
    (D) Appendix B, Error and Statistical Calculations. Table IE.
    (6) Office of Science and Technology, U.S. Environmental Protection 
Agency, Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) Method 1625C, Semivolatile Organic Compounds by Isotope 
Dilution GCMS. 1989. Table IF.
    (ii) [Reserved]
    (7) Office of Water, U.S. Environmental Protection Agency, 
Washington DC (US EPA). Available at http://water.epa.gov/scitech/methods/cwa/index.cfm or from National Technical Information Service, 
5285 Port Royal Road, Springfield, Virginia 22161.
    (i) Method 1631, Mercury in Water by Oxidation, Purge and Trap, and 
Cold Vapor Atomic Fluorescence Spectrometry. Revision E, August 2002. 
EPA-821-R-02-019, Pub. No. PB2002-108220. Table IB, Note 43.
    (ii) Kelada-01, Kelada Automated Test Methods for Total Cyanide, 
Acid Dissociable Cyanide, and Thiocyanate. Revision 1.2, August 2001. 
EPA 821-B-01-009, Pub. No. PB 2001-108275. Table IB, Note 55.
    (iii) In the compendium Analytical Methods for the Determination of 
Pollutants in Pharmaceutical Manufacturing Industry Wastewaters. July 
1998. EPA 821-B-98-016, Pub. No. PB95201679. Table IF, Note 1.
    (A) EPA Method 1666, Volatile Organic Compounds Specific to the 
Pharmaceutical Industry by Isotope Dilution GC/MS. Table IF, Note 1.
    (B) EPA Method 1667, Formaldehyde, Isobutyraldehyde, and Furfural 
by Derivatization Followed by High Performance Liquid Chromatography. 
Table IF.
    (C) Method 1671, Volatile Organic Compounds Specific to the

[[Page 29800]]

Pharmaceutical Manufacturing Industry by GC/FID. Table IF.
    (iv) Methods For The Determination of Nonconventional Pesticides In 
Municipal and Industrial Wastewater, Volume I. Revision I, August 1993. 
EPA 821-R-93-010A, Pub. No. PB 94121654. Tables ID, IG.
    (A) Method 608.1, Organochlorine Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (B) Method 608.2, Certain Organochlorine Pesticides. Table ID, Note 
10; Table IG, Note 3.
    (C) Method 614, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (D) Method 614.1, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (E) Method 615, Chlorinated Herbicides. Table ID, Note 10; Table 
IG, Note 3.
    (F) Method 617, Organohalide Pesticides and PCBs. Table ID, Note 
10; Table IG, Note 3.
    (G) Method 619, Triazine Pesticides. Table ID, Note 10; Table IG, 
Note 3.
    (H) Method 622, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (I) Method 622.1, Thiophosphate Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (J) Method 627, Dinitroaniline Pesticides. Table ID, Note 10; Table 
IG, Notes 1 and 3.
    (K) Method 629, Cyanazine. Table IG, Note 3.
    (L) Method 630, Dithiocarbamate Pesticides. Table IG, Note 3.
    (M) Method 630.1, Dithiocarbamate Pesticides. Table IG, Note 3.
    (N) Method 631, Benomyl and Carbendazim. Table IG, Note 3.
    (O) Method 632, Carbamate and Urea Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (P) Method 632.1, Carbamate and Amide Pesticides. Table IG, Note 3.
    (Q) Method 633, Organonitrogen Pesticides. Table IG, Note 3.
    (R) Method 633.1, Neutral Nitrogen-Containing Pesticides. Table IG, 
Note 3.
    (S) Method 637, MBTS and TCMTB. Table IG, Note 3.
    (T) Method 644, Picloram. Table IG, Note 3.
    (U) Method 645, Certain Amine Pesticides and Lethane. Table IG, 
Note 3.
    (V) Method 1656, Organohalide Pesticides. Table ID, Note 10; Table 
IG, Notes 1 and 3.
    (W) Method 1657, Organophosphorus Pesticides. Table ID, Note 10; 
Table IG, Note 3.
    (X) Method 1658, Phenoxy-Acid Herbicides. Table IG, Note 3.
    (Y) Method 1659, Dazomet. Table IG, Note 3.
    (Z) Method 1660, Pyrethrins and Pyrethroids. Table IG, Note 3.
    (AA) Method 1661, Bromoxynil. Table IG, Note 3.
    (BB) Ind-01. Methods EV-024 and EV-025, Analytical Procedures for 
Determining Total Tin and Triorganotin in Wastewater. Table IG, Note 3.
    (v) Methods For The Determination of Nonconventional Pesticides In 
Municipal and Industrial Wastewater, Volume II. August 1993. EPA 821-R-
93-010B, Pub. No. PB 94166311. Table IG.
    (A) Method 200.9, Determination of Trace Elements by Stabilized 
Temperature Graphite Furnace Atomic Absorption Spectrometry. Table IG, 
Note 3.
    (B) Method 505, Analysis of Organohalide Pesticides and Commercial 
Polychlorinated Biphenyl (PCB) Products in Water by Microextraction and 
Gas Chromatography. Table ID, Note 10; Table IG, Note 3.
    (C) Method 507, The Determination of Nitrogen- and Phosphorus-
Containing Pesticides in Water by Gas Chromatography with a Nitrogen-
Phosphorus Detector. Table ID, Note 10; Table IG, Note 3.
    (D) Method 508, Determination of Chlorinated Pesticides in Water by 
Gas Chromatography with an Electron Capture Detector. Table ID, Note 
10; Table IG, Note 3.
    (E) Method 515.1, Determination of Chlorinated Acids in Water by 
Gas Chromatography with an Electron Capture Detector. Table IG, Notes 2 
and 3.
    (F) Method 515.2, Determination of Chlorinated Acids in Water Using 
Liquid-Solid Extraction and Gas Chromatography with an Electron Capture 
Detector. Table IG, Notes 2 and 3.
    (G) Method 525.1, Determination of Organic Compounds in Drinking 
Water by Liquids-Solid Extraction and Capillary Column Gas 
Chromatography/Mass Spectrometry. Table ID, Note 10; Table IG, Note 3.
    (H) Method 531.1, Measurement of N-Methylcarbamoyloximes and N-
Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post-
Column Derivatization. Table ID, Note 10; Table IG, Note 3.
    (I) Method 547, Determination of Glyphosate in Drinking Water by 
Direct-Aqueous-Injection HPLC, Post-Column Derivatization, and 
Fluorescence Detection. Table IG, Note 3.
    (J) Method 548, Determination of Endothall in Drinking Water by 
Aqueous Derivatization, Liquid-Solid Extraction, and Gas Chromatography 
with Electron-Capture Detector. Table IG, Note 3.
    (K) Method 548.1, Determination of Endothall in Drinking Water by 
Ion-Exchange Extraction, Acidic Methanol Methylation and Gas 
Chromatography/Mass Spectrometry. Table IG, Note 3.
    (L) Method 553, Determination of Benzidines and Nitrogen-Containing 
Pesticides in Water by Liquid-Liquid Extraction or Liquid-Solid 
Extraction and Reverse Phase High Performance Liquid Chromatography/
Particle Beam/Mass Spectrometry Table ID, Note 10; Table IG, Note 3.
    (M) Method 555, Determination of Chlorinated Acids in Water by High 
Performance Liquid Chromatography With a Photodiode Array Ultraviolet 
Detector. Table IG, Note 3.
    (vi) In the compendium Methods for the Determination of Organic 
Compounds in Drinking Water. Revised July 1991, December 1998. EPA-600/
4-88-039, Pub. No. PB92-207703. Table IF.
    (A) EPA Method 502.2, Volatile Organic Compounds in Water by Purge 
and Trap Capillary Column Gas Chromatography with Photoionization and 
Electrolytic Conductivity Detectors in Series. Table IF.
    (B) [Reserved]
    (vii) In the compendium Methods for the Determination of Organic 
Compounds in Drinking Water-Supplement II. August 1992. EPA-600/R-92-
129, Pub. No. PB92-207703. Table IF.
    (A) EPA Method 524.2, Measurement of Purgeable Organic Compounds in 
Water by Capillary Column Gas Chromatography/Mass Spectrometry. Table 
IF.
    (B) [Reserved]
    (viii) Methods for Measuring the Acute Toxicity of Effluents and 
Receiving Waters to Freshwater and Marine Organisms, Fifth Edition. 
October 2002. EPA 821-R-02-012, Pub. No. PB2002-108488. Table IA, Note 
26.
    (ix) Short-Term Methods for Measuring the Chronic Toxicity of 
Effluents and Receiving Waters to Freshwater Organisms, Fourth Edition. 
October 2002. EPA 821-R-02-013, Pub. No. PB2002-108489. Table IA, Note 
27.
    (x) Short-Term Methods for Measuring the Chronic Toxicity of 
Effluents and Receiving Waters to Marine and Estuarine Organisms, Third 
Edition. October 2002. EPA 821-R-02-014, Pub. No. PB2002-108490. Table 
IA, Note 28.
    (8) Office of Water, U.S. Environmental Protection Agency, 
Washington DC (US EPA). Available at

[[Page 29801]]

http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (i) Method 245.7, Mercury in Water by Cold Vapor Atomic 
Fluorescence Spectrometry. Revision 2.0, February 2005. EPA-821-R-05-
001. Table IB, Note 17.
    (ii) Method 1103.1: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). 
March 2010. EPA-621-R-10-002. Table IH, Note 19.
    (iii) Method 1106.1: Enterococci in Water by Membrane Filtration 
Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). December 2009. 
EPA-621-R-09-015. Table IH, Note 23.
    (iv) Method 1600: Enterococci in Water by Membrane Filtration Using 
membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). December 
2009. EPA-821-R-09-016. Table IA, Note 25; Table IH, Note 24.
    (v) Method 1603: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar 
(Modified mTEC). December 2009. EPA-821-R-09-007. Table IA, Note 22; 
Table IH, Note 20.
    (vi) Method 1604: Total Coliforms and Escherichia coli (E. coli) in 
Water by Membrane Filtration Using a Simultaneous Detection Technique 
(MI Medium). September 2002. EPA-821-R-02-024. Table IH, Note 21.
    (vii) Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. 
December 2005. EPA-821-R-05-001. Table IH, Note 25.
    (viii) Method 1623: Cryptosporidium and Giardia in Water by 
Filtration/IMS/FA. December 2005. EPA-821-R-05-002. Table IH, Note 26.
    (ix) Method 1627, Kinetic Test Method for the Prediction of Mine 
Drainage Quality. December 2011. EPA-821-R-09-002. Table IB, Note 69.
    (x) Method 1664, n-Hexane Extractable Material (HEM; Oil and 
Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; 
Non-polar Material) by Extraction and Gravimetry. Revision A, February 
1999. EPA-821-R-98-002. Table IB, Notes 38 and 42.
    (xi) Method 1664, n-Hexane Extractable Material (HEM; Oil and 
Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; 
Non-polar Material) by Extraction and Gravimetry. Revision B, February 
2010. EPA-821-R-10-001. Table IB, Notes 38 and 42.
    (xii) Method 1669, Sampling Ambient Water for Trace Metals at EPA 
Water Quality Criteria Levels. July 1996. Table IB, Note 43.
    (xiii) Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by 
Multiple-Tube Fermentation using Lauryl Tryptose Broth (LTB) and EC 
Medium. April 2010. EPA-821-R-10-003. Table IA, Note 15.
    (xiv) Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by 
Multiple-Tube Fermentation using A-1 Medium. July 2006. EPA 821-R-06-
013. Table IA, Note 20.
    (xv) Method 1682: Salmonella in Sewage Sludge (Biosolids) by 
Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. July 2006. EPA 
821-R-06-014. Table IA, Note 23.
    (9) American National Standards Institute, 1430 Broadway, New York 
NY 10018.
    (i) ANSI. American National Standard on Photographic Processing 
Effluents. April 2, 1975. Table IB, Note 9.
    (ii) [Reserved]
    (10) American Public Health Association, 1015 15th Street NW., 
Washington, DC 20005. Standard Methods Online is available through the 
Standard Methods Web site (http://www.standardmethods.org).
    (i) Standard Methods for the Examination of Water and Wastewater. 
14th Edition, 1975. Table IB, Notes 17 and 27.
    (ii) Standard Methods for the Examination of Water and Wastewater. 
15th Edition, 1980, Table IB, Note 30; Table ID.
    (iii) Selected Analytical Methods Approved and Cited by the United 
States Environmental Protection Agency, Supplement to the 15th Edition 
of Standard Methods for the Examination of Water and Wastewater. 1981. 
Table IC, Note 6; Table ID, Note 6.
    (iv) Standard Methods for the Examination of Water and Wastewater. 
18th Edition, 1992. Tables IA, IB, IC, ID, IE, and IH.
    (v) Standard Methods for the Examination of Water and Wastewater. 
19th Edition, 1995. Tables IA, IB, IC, ID, IE, and IH.
    (vi) Standard Methods for the Examination of Water and Wastewater. 
20th Edition, 1998. Tables IA, IB, IC, ID, IE, and IH.
    (vii) Standard Methods for the Examination of Water and Wastewater. 
21st Edition, 2005. Table IB, Notes 17 and 27.
    (viii) 2120, Color. 2001. Table IB.
    (ix) 2130, Turbidity. 2001. Table IB.
    (x) 2310, Acidity. 1997. Table IB.
    (xi) 2320, Alkalinity. 1997. Table IB.
    (xii) 2340, Hardness. 1997. Table IB.
    (xiii) 2510, Conductivity. 1997. Table IB.
    (xiv) 2540, Solids. 1997. Table IB.
    (xv) 2550, Temperature. 2000. Table IB.
    (xvi) 3111, Metals by Flame Atomic Absorption Spectrometry. 1999. 
Table IB.
    (xvii) 3112, Metals by Cold-Vapor Atomic Absorption Spectrometry. 
2009. Table IB.
    (xviii) 3113, Metals by Electrothermal Atomic Absorption 
Spectrometry. 2004. Table IB.
    (xix) 3114, Arsenic and Selenium by Hydride Generation/Atomic 
Absorption Spectrometry. 2009. Table IB.
    (xx) 3120, Metals by Plasma Emission. 1999. Table IB.
    (xxi) 3125, Metals by Inductively Coupled Plasma-Mass Spectrometry. 
2009. Table IB.
    (xxii) 3500-Al, Aluminum. 2001. Table IB.
    (xxiii) 3500-As, Arsenic. 1997. Table IB.
    (xxiv) 3500-Ca, Calcium. 1997. Table IB.
    (xxv) 3500-Cr, Chromium. 2009. Table IB.
    (xxvi) 3500-Cu, Copper. 1999. Table IB.
    (xxvii) 3500-Fe, Iron. 1997. Table IB.
    (xxviii) 3500-Pb, Lead. 1997. Table IB.
    (xxix) 3500-Mn, Manganese. 1999. Table IB.
    (xxx) 3500-K, Potassium. 1997. Table IB.
    (xxxi) 3500-Na, Sodium. 1997. Table IB.
    (xxxii) 3500-V, Vanadium. 1997. Table IB.
    (xxxiii) 3500-Zn, Zinc. 1997. Table IB.
    (xxxiv) 4110, Determination of Anions by Ion Chromatography. 2000. 
Table IB.
    (xxxv) 4140, Inorganic Anions by Capillary Ion Electrophoresis. 
1997. Table IB.
    (xxxvi) 4500-B, Boron. 2000. Table IB.
    (xxxvii) 4500-Cl-, Chloride. 1997. Table IB.
    (xxxviii) 4500-Cl, Chlorine (Residual). 2000. Table IB.
    (xxxix) 4500-CN-, Cyanide. 1999. Table IB.
    (xl) 4500-F-, Fluoride. 1997. Table IB.
    (xli) 4500-H\+\, pH Value. 2000. Table IB.
    (xlii) 4500-NH3, Nitrogen (Ammonia). 1997. Table IB.
    (xliii) 4500-NO2-, Nitrogen (Nitrite). 2000. 
Table IB.
    (xliv) 4500-NO3-, Nitrogen (Nitrate). 2000. 
Table IB.
    (xlv) 4500-Norg, Nitrogen (Organic). 1997. Table IB.
    (xlvi) 4500-O, Oxygen (Dissolved). 2001. Table IB.
    (xlvii) 4500-P, Phosphorus. 1999. Table IB.
    (xlviii) 4500-SiO2, Silica. 1997. Table IB.

[[Page 29802]]

    (xlix) 4500-S2-, Sulfide. 2000. Table IB.
    (l) 4500-SO32-, Sulfite. 2000. Table IB.
    (li) 4500-SO42-, Sulfate. 1997. Table IB.
    (lii) 5210, Biochemical Oxygen Demand (BOD). 2001. Table IB.
    (liii) 5220, Chemical Oxygen Demand (COD). 1997. Table IB.
    (liv) 5310, Total Organic Carbon (TOC). 2000. Table IB.
    (lv) 5520, Oil and Grease. 2001. Table IB.
    (lvi) 5530, Phenols. 2005. Table IB.
    (lvii) 5540, Surfactants. 2000. Table IB.
    (lviii) 6200, Volatile Organic Compounds. 1997. Table IC.
    (lix) 6410, Extractable Base/Neutrals and Acids. 2000. Tables IC, 
ID.
    (lx) 6420, Phenols. 2000. Table IC.
    (lxi) 6440, Polynuclear Aromatic Hydrocarbons. 2000. Table IC.
    (lxii) 6630, Organochlorine Pesticides. 2000. Table ID.
    (lxiii) 6640, Acidic Herbicide Compounds. 2001. Table ID.
    (lxiv) 7110, Gross Alpha and Gross Beta Radioactivity (Total, 
Suspended, and Dissolved). 2000. Table IE.
    (lxv) 7500, Radium. 2001. Table IE.
    (lxvi) 9213, Recreational Waters. 2007. Table IH.
    (lxvii) 9221, Multiple-Tube Fermentation Technique for Members of 
the Coliform Group. 2006. Table IA, Notes 12 and 14; Table IH, Notes 11 
and 13.
    (lxviii) 9222, Membrane Filter Technique for Members of the 
Coliform Group. 1997. Table IA; Table IH, Note 18.
    (lxix) 9223, Enzyme Substrate Coliform Test. 2004. Table IA; Table 
IH.
    (lxx) 9230, Fecal Enterococcus/Streptococcus Groups. 2007. Table 
IA; Table IH.
    (11) The Analyst, The Royal Society of Chemistry, RSC Publishing, 
Royal Society of Chemistry, Thomas Graham House, Science Park, Milton 
Road, Cambridge CB4 0WF, United Kingdom. (Also available from most 
public libraries.)
    (i) Spectrophotometric Determination of Ammonia: A Study of a 
Modified Berthelot Reaction Using Salicylate and Dichloroisocyanurate. 
Krom, M.D. 105:305-316, April 1980. Table IB, Note 60.
    (ii) [Reserved]
    (12) Analytical Chemistry, ACS Publications, 1155 Sixteenth St. 
NW., Washington DC 20036. (Also available from most public libraries.)
    (i) Spectrophotometric and Kinetics Investigation of the Berthelot 
Reaction for the Determination of Ammonia. Patton, C.J. and S.R. 
Crouch. 49(3):464-469, March 1977. Table IB, Note 60.
    (ii) [Reserved]
    (13) AOAC International, 481 North Frederick Avenue, Suite 500, 
Gaithersburg, MD 20877-2417.
    (i) Official Methods of Analysis of AOAC International. 16th 
Edition, 4th Revision, 1998.
    (A) 920.203, Manganese in Water, Persulfate Method. Table IB, Note 
3.
    (B) 925.54, Sulfate in Water, Gravimetric Method. Table IB, Note 3.
    (C) 973.40, Specific Conductance of Water. Table IB, Note 3.
    (D) 973.41, pH of Water. Table IB, Note 3.
    (E) 973.43, Alkalinity of Water, Titrimetric Method. Table IB, Note 
3.
    (F) 973.44, Biochemical Oxygen Demand (BOD) of Water, Incubation 
Method. Table IB, Note 3.
    (G) 973.45, Oxygen (Dissolved) in Water, Titrimetric Methods. Table 
IB, Note 3.
    (H) 973.46, Chemical Oxygen Demand (COD) of Water, Titrimetric 
Methods. Table IB, Note 3.
    (I) 973.47, Organic Carbon in Water, Infrared Analyzer Method. 
Table IB, Note 3.
    (J) 973.48, Nitrogen (Total) in Water, Kjeldahl Method. Table IB, 
Note 3.
    (K) 973.49, Nitrogen (Ammonia) in Water, Colorimetric Method. Table 
IB, Note 3.
    (L) 973.50, Nitrogen (Nitrate) in Water, Brucine Colorimetric 
Method. Table IB, Note 3.
    (M) 973.51, Chloride in Water, Mercuric Nitrate Method. Table IB, 
Note 3.
    (N) 973.52, Hardness of Water. Table IB, Note 3.
    (O) 973.53, Potassium in Water, Atomic Absorption 
Spectrophotometric Method. Table IB, Note 3.
    (P) 973.54, Sodium in Water, Atomic Absorption Spectrophotometric 
Method. Table IB, Note 3.
    (Q) 973.55, Phosphorus in Water, Photometric Method. Table IB, Note 
3.
    (R) 973.56, Phosphorus in Water, Automated Method. Table IB, Note 
3.
    (S) 974.27, Cadmium, Chromium, Copper, Iron, Lead, Magnesium, 
Manganese, Silver, Zinc in Water, Atomic Absorption Spectrophotometric 
Method. Table IB, Note 3.
    (T) 977.22, Mercury in Water, Flameless Atomic Absorption 
Spectrophotometric Method. Table IB, Note 3.
    (U) 991.15. Total Coliforms and Escherichia coli in Water Defined 
Substrate Technology (Colilert) Method. Table IA, Note 10; Table IH, 
Note 10.
    (V) 993.14, Trace Elements in Waters and Wastewaters, Inductively 
Coupled Plasma-Mass Spectrometric Method. Table IB, Note 3.
    (W) 993.23, Dissolved Hexavalent Chromium in Drinking Water, Ground 
Water, and Industrial Wastewater Effluents, Ion Chromatographic Method. 
Table IB, Note 3.
    (X) 993.30, Inorganic Anions in Water, Ion Chromatographic Method. 
Table IB, Note 3.
    (ii) [Reserved]
    (14) Applied and Environmental Microbiology, American Society for 
Microbiology, 1752 N Street NW., Washington DC 20036. (Also available 
from most public libraries.)
    (i) New Medium for the Simultaneous Detection of Total Coliforms 
and Escherichia coli in Water. Brenner, K.P., C.C. Rankin, Y.R. Roybal, 
G.N. Stelma, Jr., P.V. Scarpino, and A.P. Dufour. 59:3534-3544, 
November 1993. Table IH, Note 21.
    (ii) [Reserved]
    (15) ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West 
Conshohocken, PA 19428-2959, or online at http://www.astm.org.
    (i) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1994. Tables IA, IB, 
IC, ID, IE, and IH.
    (ii) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1996. Tables IA, IB, 
IC, ID, IE, and IH.
    (iii) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 1999. Tables IA, IB, 
IC, ID, IE, and IH.
    (iv) Annual Book of ASTM Standards, Water, and Environmental 
Technology, Section 11, Volumes 11.01 and 11.02. 2000. Tables IA, IB, 
IC, ID, IE, and IH.
    (v) ASTM D511-08, Standard Test Methods for Calcium and Magnesium 
in Water. November 2008. Table IB.
    (vi) ASTM D512-04, Standard Test Methods for Chloride Ion in Water. 
July 2004. Table IB.
    (vii) ASTM D515-88, Test Methods for Phosphorus in Water, March 
1989. Table IB.
    (viii) ASTM D516-07, Standard Test Method for Sulfate Ion in Water, 
September 2007. Table IB.
    (ix) ASTM D858-07, Standard Test Methods for Manganese in Water. 
August 2007. Table IB.
    (x) ASTM D859-05, Standard Test Method for Silica in Water. 
February 2005. Table IB.
    (xi) ASTM D888-09, Standard Test Methods for Dissolved Oxygen in 
Water. December 2009. Table IB.
    (xii) ASTM D1067-06, Standard Test Methods for Acidity or 
Alkalinity of Water. January 2007. Table IB.

[[Page 29803]]

    (xiii) ASTM D1068-05\E1\, Standard Test Methods for Iron in Water. 
July 2005. Table IB.
    (xiv) ASTM D1125-95 (Reapproved 1999), Standard Test Methods for 
Electrical Conductivity and Resistivity of Water. December 1995. Table 
IB.
    (xv) ASTM D1126-02 (Reapproved 2007)\E1\, Standard Test Method for 
Hardness in Water. August 2007. Table IB.
    (xvi) ASTM D1179-04, Standard Test Methods for Fluoride Ion in 
Water. July 2004. Table IB.
    (xvii) ASTM D1246-05, Standard Test Method for Bromide Ion in 
Water. February 2005. Table IB.
    (xviii) ASTM D1252-06, Standard Test Methods for Chemical Oxygen 
Demand (Dichromate Oxygen Demand) of Water. February 2006. Table IB.
    (xix) ASTM D1253-08, Standard Test Method for Residual Chlorine in 
Water. October 2008. Table IB.
    (xx) ASTM D1293-99, Standard Test Methods for pH of Water. March 
2000. Table IB.
    (xxi) ASTM D1426-08, Standard Test Methods for Ammonia Nitrogen in 
Water. September 2008. Table IB.
    (xxii) ASTM D1687-02 (Reapproved 2007)\E1\, Standard Test Methods 
for Chromium in Water. August 2007. Table IB.
    (xxiii) ASTM D1688-07, Standard Test Methods for Copper in Water. 
August 2007. Table IB.
    (xxiv) ASTM D1691-02 (Reapproved 2007)\E1\, Standard Test Methods 
for Zinc in Water. August 2007. Table IB.
    (xxv) ASTM D1783-01 (Reapproved 2007), Standard Test Methods for 
Phenolic Compounds in Water. January 2008). Table IB.
    (xxvi) ASTM D1886-08, Standard Test Methods for Nickel in Water. 
October 2008. Table IB.
    (xxvii) ASTM D1889-00, Standard Test Method for Turbidity of Water. 
October 2000. Table IB.
    (xxviii) ASTM D1890-96, Standard Test Method for Beta Particle 
Radioactivity of Water. April 1996. Table IE.
    (xxix) ASTM D1943-96, Standard Test Method for Alpha Particle 
Radioactivity of Water. April 1996. Table IE.
    (xxx) ASTM D1976-07, Standard Test Method for Elements in Water by 
Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy. August 
2007. Table IB.
    (xxxi) ASTM D2036-09, Standard Test Methods for Cyanides in Water. 
October 2009. Table IB.
    (xxxii) ASTM D2330-02, Standard Test Method for Methylene Blue 
Active Substances. August 2002. Table IB.
    (xxxiii) ASTM D2460-97, Standard Test Method for Alpha-Particle-
Emitting Isotopes of Radium in Water. October 1997. Table IE.
    (xxxiv) ASTM D2972-08, Standard Tests Method for Arsenic in Water. 
October 2008. Table IB.
    (xxxv) ASTM D3223-02 (Reapproved 2007)\E1\, Standard Test Method 
for Total Mercury in Water. August 2007. Table IB.
    (xxxvi) ASTM D3371-95, Standard Test Method for Nitriles in Aqueous 
Solution by Gas-Liquid Chromatography, February 1996. Table IF.
    (xxxvii) ASTM D3373-03 (Reapproved 2007)\E1\, Standard Test Method 
for Vanadium in Water. September 2007. Table IB.
    (xxxviii) ASTM D3454-97, Standard Test Method for Radium-226 in 
Water. February 1998. Table IE.
    (xxxix) ASTM D3557-02 (Reapproved 2007)\E1\, Standard Test Method 
for Cadmium in Water. September 2007. Table IB.
    (xl) ASTM D3558-08, Standard Test Method for Cobalt in Water. 
November 2008. Table IB.
    (xli) ASTM D3559-08, Standard Test Methods for Lead in Water. 
October 2008. Table IB.
    (xlii) ASTM D3590-02 (Reapproved 2006), Standard Test Methods for 
Total Kjeldahl Nitrogen in Water. February 2007. Table IB.
    (xliii) ASTM D3645-08, Standard Test Methods for Beryllium in 
Water. October 2008. Table IB.
    (xliv) ASTM D3695-95, Standard Test Method for Volatile Alcohols in 
Water by Direct Aqueous-Injection Gas Chromatography. April 1995. Table 
IF.
    (xlv) ASTM D3859-08, Standard Test Methods for Selenium in Water. 
October 2008. Table IB.
    (xlvi) ASTM D3867-04, Standard Test Method for Nitrite-Nitrate in 
Water. July 2004. Table IB.
    (xlvii) ASTM D4190-08, Standard Test Method for Elements in Water 
by Direct-Current Plasma Atomic Emission Spectroscopy. October 2008. 
Table IB.
    (xlviii) ASTM D4282-02, Standard Test Method for Determination of 
Free Cyanide in Water and Wastewater by Microdiffusion. August 2002. 
Table IB.
    (xlix) ASTM D4327-03, Standard Test Method for Anions in Water by 
Chemically Suppressed Ion Chromatography. January 2003. Table IB.
    (l) ASTM D4382-02 (Reapproved 2007)\E1\, Standard Test Method for 
Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace. 
September 2007. Table IB.
    (li) ASTM D4657-92 (Reapproved 1998), Standard Test Method for 
Polynuclear Aromatic Hydrocarbons in Water. January 1993. Table IC.
    (lii) ASTM D4658-08, Standard Test Method for Sulfide Ion in Water. 
August 2008. Table IB.
    (liii) ASTM D4763-88 (Reapproved 2001), Standard Practice for 
Identification of Chemicals in Water by Fluorescence Spectroscopy. 
September 1988. Table IF.
    (liv) ASTM D4839-03, Standard Test Method for Total Carbon and 
Organic Carbon in Water by Ultraviolet, or Persulfate Oxidation, or 
Both, and Infrared Detection. January 2003. Table IB.
    (lv) ASTM D5257-03, Standard Test Method for Dissolved Hexavalent 
Chromium in Water by Ion Chromatography. January 2003. Table IB.
    (lvi) ASTM D5259-92, Standard Test Method for Isolation and 
Enumeration of Enterococci from Water by the Membrane Filter Procedure. 
October 1992. Table IH, Note 9.
    (lvii) ASTM D5392-93, Standard Test Method for Isolation and 
Enumeration of Escherichia coli in Water by the Two-Step Membrane 
Filter Procedure. September 1993. Table IH, Note 9.
    (lviii) ASTM D5673-05, Standard Test Method for Elements in Water 
by Inductively Coupled Plasma--Mass Spectrometry. July 2005. Table IB.
    (lix) ASTM D5907-03, Standard Test Method for Filterable and 
Nonfilterable Matter in Water. July 2003. Table IB.
    (lx) ASTM D6503-99, Standard Test Method for Enterococci in Water 
Using Enterolert. April 2000. Table IA Note 9, Table IH, Note 9.
    (lxi) ASTM. D6508-00 (Reapproved 2005)\E2\, Standard Test Method 
for Determination of Dissolved Inorganic Anions in Aqueous Matrices 
Using Capillary Ion Electrophoresis and Chromate Electrolyte. April 
2005. Table IB.
    (lxii) ASTM. D6888-09, Standard Test Method for Available Cyanide 
with Ligand Displacement and Flow Injection Analysis (FIA) Utilizing 
Gas Diffusion Separation and Amperometric Detection. October 2009. 
Table IB, Note 59.
    (lxiii) ASTM. D6919-09, Standard Test Method for Determination of 
Dissolved Alkali and Alkaline Earth Cations and Ammonium in Water and 
Wastewater by Ion Chromatography. May 2009. Table IB.
    (lxiv) ASTM. D7065-06, Standard Test Method for Determination of 
Nonylphenol, Bisphenol A, p-tert-Octylphenol, Nonylphenol 
Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters

[[Page 29804]]

by Gas Chromatography Mass Spectrometry. January 2007. Table IC.
    (lxv) ASTM. D7237-10, Standard Test Method for Free Cyanide with 
Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and 
Amperometric Detection. June 2010. Table IB.
    (lxvi) ASTM. D7284-08, Standard Test Method for Total Cyanide in 
Water by Micro Distillation followed by Flow Injection Analysis with 
Gas Diffusion Separation and Amperometric Detection. April 2008). Table 
IB.
    (lxvii) ASTM. D7365-09a, Standard Practice for Sampling, 
Preservation, and Mitigating Interferences in Water Samples for 
Analysis of Cyanide. October 2009. Table II, Notes 5 and 6.
    (lxviii) ASTM. D7511-09\E2\, Standard Test Method for Total Cyanide 
by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and 
Amperometric Detection. March 2009. Table IB.
    (lxix) ASTM. D7573-09, Standard Test Method for Total Carbon and 
Organic Carbon in Water by High Temperature Catalytic Combustion and 
Infrared Detection. November 2009. Table IB.
    (16) Bran & Luebbe Analyzing Technologies, Inc., Elmsford NY 10523.
    (i) Industrial Method Number 378-75WA, Hydrogen Ion (pH) Automated 
Electrode Method, Bran & Luebbe (Technicon) Auto Analyzer II. October 
1976. Table IB, Note 21.
    (ii) [Reserved]
    (17) CEM Corporation, P.O. Box 200, Matthews NC 28106-0200.
    (i) Closed Vessel Microwave Digestion of Wastewater Samples for 
Determination of Metals. April 16, 1992. Table IB, Note 36.
    (ii) [Reserved]
    (18) Craig R. Chinchilla, 900 Jorie Blvd., Suite 35, Oak Brook IL 
60523. Telephone: 630-645-0600.
    (i) Nitrate by Discrete Analysis Easy (1-Reagent) Nitrate Method, 
(Colorimetric, Automated, 1 Reagent). Revision 1, November 12, 2011. 
Table IB, Note 62.
    (ii) [Reserved]
    (19) Hach Company, P.O. Box 389, Loveland CO 80537.
    (i) Method 8000, Chemical Oxygen Demand. Hach Handbook of Water 
Analysis. 1979. Table IB, Note 14.
    (ii) Method 8008, 1,10-Phenanthroline Method using FerroVer Iron 
Reagent for Water. 1980. Table IB, Note 22.
    (iii) Method 8009, Zincon Method for Zinc. Hach Handbook for Water 
Analysis. 1979. Table IB, Note 33.
    (iv) Method 8034, Periodate Oxidation Method for Manganese. Hach 
Handbook for Water Analysis. 1979. Table IB, Note 23.
    (v) Method 8506, Bicinchoninate Method for Copper. Hach Handbook of 
Water Analysis. 1979. Table IB, Note 19.
    (vi) Method 8507, Nitrogen, Nitrite--Low Range, Diazotization 
Method for Water and Wastewater. 1979. Table IB, Note 25.
    (vii) Hach Method 10360, Luminescence Measurement of Dissolved 
Oxygen in Water and Wastewater and for Use in the Determination of 
BOD5 and cBOD5. Revision 1.2, October 2011. Table 
IB, Note 63.
    (viii) m-ColiBlue24[supreg] Method, for total Coliforms and E. 
coli. Revision 2, 1999. Table IA, Note 18; Table IH, Note 17.
    (20) IDEXX Laboratories Inc., One Idexx Drive, Westbrook ME 04092.
    (i) Colilert[supreg] Method. 2002. Table IA, Notes 17 and 18; Table 
IH, Notes 14, 15 and 16.
    (ii) Colilert-18[supreg] Method. 2002. Table IA, Notes 17 and 18; 
Table IH, Notes 14, 15 and 16.
    (iii) Enterolert[supreg] Method. 2002. Table IA, Note 24; Table IH, 
Note 12.
    (iv) Quanti-Tray[supreg] Method. 2002. Table IA, Note 18; Table IH, 
Notes 14 and 16.
    (v) Quanti-Tray[supreg]/2000 Method. 2002. Table IA, Note 18; Table 
IH, Notes 14 and 16.
    (21) In-Situ Incorporated, 221 E. Lincoln Ave., Ft. Collins CO 
80524. Telephone: 970-498-1500.
    (i) In-Situ Inc. Method 1002-8-2009, Dissolved Oxygen Measurement 
by Optical Probe. 2009. Table IB, Note 64.
    (ii) In-Situ Inc. Method 1003-8-2009, Biochemical Oxygen Demand 
(BOD) Measurement by Optical Probe. 2009. Table IB, Note 10.
    (iii) In-Situ Inc. Method 1004-8-2009, Carbonaceous Biochemical 
Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. Table IB, Note 
35.
    (22) Journal of Chromatography, Elsevier/North-Holland, Inc., 
Journal Information Centre, 52 Vanderbilt Avenue, New York NY 10164. 
(Also available from most public libraries.
    (i) Direct Determination of Elemental Phosphorus by Gas-Liquid 
Chromatography. Addison, R.F. and R.G. Ackman. 47(3): 421-426, 1970. 
Table IB, Note 28.
    (ii) [Reserved]
    (23) Lachat Instruments, 6645 W. Mill Road, Milwaukee WI 53218, 
Telephone: 414-358-4200.
    (i) QuikChem Method 10-204-00-1-X, Digestion and Distillation of 
Total Cyanide in Drinking and Wastewaters using MICRO DIST and 
Determination of Cyanide by Flow Injection Analysis. Revision 2.2, 
March 2005. Table IB, Note 56.
    (ii) [Reserved]
    (24) Leck Mitchell, Ph.D., P.E., 656 Independence Valley Dr., Grand 
Junction CO 81507. Telephone: 970-244-8661.
    (i) Mitchell Method M5271, Determination of Turbidity by 
Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 66.
    (ii) Mitchell Method M5331, Determination of Turbidity by 
Nephelometry. Revision 1.0, July 31, 2008. Table IB, Note 65.
    (25) National Council of the Paper Industry for Air and Stream 
Improvements, Inc. (NCASI), 260 Madison Avenue, New York NY 10016.
    (i) NCASI Technical Bulletin No. 253, An Investigation of Improved 
Procedures for Measurement of Mill Effluent and Receiving Water Color. 
December 1971. Table IB, Note 18.
    (ii) [Reserved]
    (26) Oceanography International Corporation, 512 West Loop, P.O. 
Box 2980, College Station TX 77840.
    (i) OIC Chemical Oxygen Demand Method. 1978. Table IB, Note 13.
    (ii) [Reserved]
    (27) OI Analytical, Box 9010, College Station TX 77820-9010.
    (i) Method OIA-1677-09, Available Cyanide by Ligand Exchange and 
Flow Injection Analysis (FIA). Copyright 2010. Table IB, Note 59.
    (ii) Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, 
Steam Distillation, Titrimetric Detection. Revised December 22, 1994. 
Table IB, Note 39.
    (iii) Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, 
Steam Distillation, Colorimetric Detection. Revised December 22, 1994. 
Table IB, Note 40.
    (iv) Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, 
Automated FIA Gas Diffusion. Revised December 22, 1994. Table IB, Note 
41.
    (28) ORION Research Corporation, 840 Memorial Drive, Cambridge, 
Massachusetts 02138.
    (i) ORION Research Instruction Manual, Residual Chlorine Electrode 
Model 97-70. 1977. Table IB, Note 16.
    (ii) [Reserved]
    (29) Technicon Industrial Systems, Tarrytown NY 10591.
    (i) Industrial Method Number 379-75WE Ammonia, Automated Electrode 
Method, Technicon Auto Analyzer II. February 19, 1976. Table IB, Note 
7.
    (ii) [Reserved]
    (30) Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin MA 
02038.
    (i) Method AES0029. Direct Current Plasma (DCP) Optical Emission 
Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 
1986, Revised 1991. Table IB, Note 34.

[[Page 29805]]

    (ii) [Reserved]
    (31) Thermo Scientific, 166 Cummings Center, Beverly MA 01915. 
Telephone: 1-800-225-1480. www.thermoscientific.com.
    (i) Thermo Scientific Orion Method AQ4500, Determination of 
Turbidity by Nephelometry. Revision 5, March 12, 2009. Table IB, Note 
67.
    (ii) [Reserved]
    (32) 3M Corporation, 3M Center Building 220-9E-10, St. Paul MN 
55144-1000.
    (i) Organochlorine Pesticides and PCBs in Wastewater Using 
Empore\TM\ Disk'' Test Method 3M 0222. Revised October 28, 1994. Table 
IC, Note 8; Table ID, Note 8.
    (ii) [Reserved]
    (33) U.S. Geological Survey (USGS), U.S. Department of the 
Interior, Reston, Virginia. Available from USGS Books and Open-File 
Reports (OFR) Section, Federal Center, Box 25425, Denver, CO 80225.
    (i) OFR 76-177, Selected Methods of the U.S. Geological Survey of 
Analysis of Wastewaters. 1976. Table IE, Note 2.
    (ii) OFR 91-519, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Organonitrogen 
Herbicides in Water by Solid-Phase Extraction and Capillary-Column Gas 
Chromatography/Mass Spectrometry With Selected-Ion Monitoring. 1992. 
Table ID, Note 14.
    (iii) OFR 92-146, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Total Phosphorus by 
a Kjeldahl Digestion Method and an Automated Colorimetric Finish That 
Includes Dialysis. 1992. Table IB, Note 48.
    (iv) OFR 93-125, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Inorganic and 
Organic Constituents in Water and Fluvial Sediments. 1993. Table IB, 
Note 51; Table IC, Note 9.
    (v) OFR 93-449, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Chromium in Water 
by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. Table 
IB, Note 46.
    (vi) OFR 94-37, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Triazine and Other 
Nitrogen-containing Compounds by Gas Chromatography with Nitrogen 
Phosphorus Detectors. 1994. Table ID, Note 9.
    (vii) OFR 95-181, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Pesticides in Water 
by C-18 Solid-Phase Extraction and Capillary-Column Gas Chromatography/
Mass Spectrometry With Selected-Ion Monitoring. 1995. Table ID, Note 
11.
    (viii) OFR 97-198, Methods of Analysis by the U.S. Geological 
Survey National Water Quality Laboratory--Determination of Molybdenum 
in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. 
Table IB, Note 47.
    (ix) OFR 98-165, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Elements in Whole-
Water Digests Using Inductively Coupled Plasma-Optical Emission 
Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. 
Table IB, Note 50.
    (x) OFR 98-639, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Arsenic and 
Selenium in Water and Sediment by Graphite Furnace--Atomic Absorption 
Spectrometry. 1999. Table IB, Note 49.
    (xi) OFR 00-170, Methods of Analysis by the U.S. Geological Survey 
National Water Quality Laboratory--Determination of Ammonium Plus 
Organic Nitrogen by a Kjeldahl Digestion Method and an Automated 
Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. 
Table IB, Note 45.
    (xii) Water-Resources Investigation Report 01-4098, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Moderate-Use Pesticides and Selected 
Degradates in Water by C-18 Solid-Phase Extraction and Gas 
Chromatography/Mass Spectrometry. 2001. Table ID, Note 13.
    (xiii) Water-Resources Investigations Report 01-4132, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Organic Plus Inorganic Mercury in Filtered 
and Unfiltered Natural Water With Cold Vapor-Atomic Fluorescence 
Spectrometry. 2001. Table IB, Note 71.
    (xiv) Water-Resources Investigation Report 01-4134, Methods of 
Analysis by the U.S. Geological Survey National Water Quality 
Laboratory--Determination of Pesticides in Water by Graphitized Carbon-
Based Solid-Phase Extraction and High-Performance Liquid 
Chormatography/Mass Spectrometry. 2001. Table ID, Note 12.
    (xv) Methods for Determination of Inorganic Substances in Water and 
Fluvial Sediments, editors, Techniques of Water-Resources 
Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. 
Table IB, Note 8.
    (xvi) Methods for Determination of Inorganic Substances in Water 
and Fluvial Sediments, Techniques of Water-Resources Investigations of 
the U.S. Geological Survey, Book 5, Chapter A1. 1989. Table IB, Note 2.
    (xvii) Methods for the Determination of Organic Substances in Water 
and Fluvial Sediments. Techniques of Water-Resources Investigations of 
the U.S. Geological Survey, Book 5, Chapter A3. 1987. Table IB, Note 
24; Table ID, Note 4.
    (xviii) Techniques and Methods Book 5-B1, Determination of Elements 
in Natural-Water, Biota, Sediment and Soil Samples Using Collision/
Reaction Cell Inductively Coupled Plasma-Mass Spectrometry. Chapter 1, 
Section B, Methods of the National Water Quality Laboratory, Book 5, 
Laboratory Analysis. 2006. Table IB, Note 70.
    (xix) U.S. Geological Survey Techniques of Water-Resources 
Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for 
Collection and Analysis of Aquatic Biological and Microbiological 
Samples. 1989. Table IA, Note 4; Table IH, Note 4.
    (xx) Water Temperature--Influential Factors, Field Measurement and 
Data Presentation, Techniques of Water-Resources Investigations of the 
U.S. Geological Survey, Book 1, Chapter D1. 1975. Table IB, Note 32.
    (34) Waters Corporation, 34 Maple Street, Milford MA 01757, 
Telephone: 508-482-2131, Fax: 508-482-3625.
    (i) Method D6508, Test Method for Determination of Dissolved 
Inorganic Anions in Aqueous Matrices Using Capillary Ion 
Electrophoresis and Chromate Electrolyte. Revision 2, December 2000. 
Table IB, Note 54.
    (ii) [Reserved]
* * * * *
    (e) Sample preservation procedures, container materials, and 
maximum allowable holding times for parameters are cited in Tables IA, 
IB, IC, ID, IE, IF, IG, and IH are prescribed in Table II. Information 
in the table takes precedence over information in specific methods or 
elsewhere. Any person may apply for a change from the prescribed 
preservation techniques, container materials, and maximum holding times 
applicable to samples taken from a specific discharge. Applications for 
such limited use changes may be made by letters to the Regional 
Alternative Test Procedure (ATP) Program Coordinator or the permitting 
authority in the Region in which the discharge will occur. Sufficient 
data should be

[[Page 29806]]

provided to assure such changes in sample preservation, containers or 
holding times do not adversely affect the integrity of the sample. The 
Regional ATP Coordinator or permitting authority will review the 
application and then notify the applicant and the appropriate State 
agency of approval or rejection of the use of the alternate test 
procedure. A decision to approve or deny any request on deviations from 
the prescribed Table II requirements will be made within 90 days of 
receipt of the application by the Regional Administrator. An analyst 
may not modify any sample preservation and/or holding time requirements 
of an approved method unless the requirements of this section are met.

                    Table II--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
                                                                                           Maximum holding time
        Parameter number/name               Container \1\          Preservation \2,3\              \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacterial Tests:
    1-5. Coliform, total, fecal, and   PA, G..................  Cool, <10 [deg]C,        8 hours.22,23
     E. coli.                                                    0.0008% Na2S2O3\ 5\.
    6. Fecal streptococci............  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.0008% Na2S2O3\ 5\.
    7. Enterococci...................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.0008% Na2S2O3\ 5\.
    8. Salmonella....................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.0008% Na2S2O3\ 5\.
Table IA--Aquatic Toxicity Tests:
    9-12. Toxicity, acute and chronic  P, FP, G...............  Cool, <=6 [deg]C \16\..  36 hours.
Table IB--Inorganic Tests:
    1. Acidity.......................  P, FP, G...............  Cool, <=6 [deg]C \18\..  14 days.
    2. Alkalinity....................  P, FP, G...............  Cool, <=6 [deg]C \18\..  14 days.
    4. Ammonia.......................  P, FP, G...............  Cool, <=6 [deg]C \18\,   28 days.
                                                                 H2SO4 to pH <2.
    9. Biochemical oxygen demand.....  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    10. Boron........................  P, FP, or Quartz.......  HNO3 to pH <2..........  6 months.
    11. Bromide......................  P, FP, G...............  None required..........  28 days.
    14. Biochemical oxygen demand,     P, FP G................  Cool, <=6 [deg]C \18\..  48 hours.
     carbonaceous.
    15. Chemical oxygen demand.......  P, FP, G...............  Cool, <=6 [deg]C \18\,   28 days.
                                                                 H2SO4 to pH <2.
    16. Chloride.....................  P, FP, G...............  None required..........  28 days.
    17. Chlorine, total residual.....  P, G...................  None required..........  Analyze within 15
                                                                                          minutes.
    21. Color........................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    23-24. Cyanide, total or           P, FP, G...............  Cool, <=6 [deg]C \18\,   14 days.
     available (or CATC) and free.                               NaOH to pH >10 5,6,
                                                                 reducing agent if
                                                                 oxidizer present.
    25. Fluoride.....................  P......................  None required..........  28 days.
    27. Hardness.....................  P, FP, G...............  HNO3 or H2SO4 to pH <2.  6 months.
    28. Hydrogen ion (pH)............  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
    31, 43. Kjeldahl and organic N...  P, FP, G...............  Cool, <=6 [deg]C\18\,    28 days.
                                                                 H2SO4 to pH <2.
Table IB--Metals: \7\
    18. Chromium VI..................  P, FP, G...............  Cool, <=6 [deg]C\18\,    28 days.
                                                                 pH = 9.3-9.7 \20\.
    35. Mercury (CVAA)...............  P, FP, G...............  HNO3 to pH <2..........  28 days.
    35. Mercury (CVAFS)..............  FP, G; and FP-lined cap  5 mL/L 12N HCl or 5 mL/  90 days.\17\
                                        \17\.                    L BrCl \17\.
    3, 5-8, 12, 13, 19, 20, 22, 26,    P, FP, G...............  HNO3 to pH <2, or at     6 months.
     29, 30, 32-34, 36, 37, 45, 47,                              least 24 hours prior
     51, 52, 58-60, 62, 63, 70-72,                               to analysis \19\.
     74, 75. Metals, except boron,
     chromium VI, and mercury.
    38. Nitrate......................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    39. Nitrate-nitrite..............  P, FP, G...............  Cool, <=6 [deg]C\18\,    28 days.
                                                                 H2SO4 to pH <2.
    40. Nitrite......................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    41. Oil and grease...............  G......................  Cool to <=6 [deg]C\18\,  28 days.
                                                                 HCl or H2SO4 to pH <2.
    42. Organic Carbon...............  P, FP, G...............  Cool to <=6 [deg]C       28 days.
                                                                 \18\, HCl, H2SO4, or
                                                                 H3PO4 to pH <2.
    44. Orthophosphate...............  P, FP, G...............  Cool, to <=6 [deg]C      Filter within 15
                                                                 \18,24\.                 minutes; Analyze
                                                                                          within 48 hours.
    46. Oxygen, Dissolved Probe......  G, Bottle and top......  None required..........  Analyze within 15
                                                                                          minutes.
    47. Winkler......................  G, Bottle and top......  Fix on site and store    8 hours.
                                                                 in dark.
    48. Phenols......................  G......................  Cool, <=6 [deg]C\18\,    28 days.
                                                                 H2SO4 to pH <2.
    49. Phosphorous (elemental)......  G......................  Cool, <=6 [deg]C \18\..  48 hours.
    50. Phosphorous, total...........  P, FP, G...............  Cool, <=6 [deg]C \18\,   28 days.
                                                                 H2SO4 to pH <2.
    53. Residue, total...............  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
    54. Residue, Filterable..........  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.

[[Page 29807]]

 
    55. Residue, Nonfilterable (TSS).  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
    56. Residue, Settleable..........  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    57. Residue, Volatile............  P, FP, G...............  Cool, <=6 [deg]C \18\..  7 days.
    61. Silica.......................  P or Quartz............  Cool, <=6 [deg]C \18\..  28 days.
    64. Specific conductance.........  P, FP, G...............  Cool, <=6 [deg]C \18\..  28 days.
    65. Sulfate......................  P, FP, G...............  Cool, <=6 [deg]C \18\..  28 days.
    66. Sulfide......................  P, FP, G...............  Cool, <=6 [deg]C \18\,   7 days.
                                                                 add zinc acetate plus
                                                                 sodium hydroxide to pH
                                                                 >9.
    67. Sulfite......................  P, FP, G...............  None required..........  Analyze within 15
                                                                                          minutes.
    68. Surfactants..................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
    69. Temperature..................  P, FP, G...............  None required..........  Analyze.
    73. Turbidity....................  P, FP, G...............  Cool, <=6 [deg]C \18\..  48 hours.
Table IC--Organic Tests: \8\
    13, 18-20, 22, 24-28, 34-37, 39-   G, FP-lined septum.....  Cool, <=6 [deg]C \18\,   14 days.
     43, 45-47, 56, 76, 104, 105, 108-                           0.008% Na2S2O3\5\.
     111, 113. Purgeable Halocarbons.
    6, 57, 106. Purgeable aromatic     G, FP-lined septum.....  Cool, <=6 [deg]C\18\,    14 days.\9\
     hydrocarbons.                                               0.008% Na2S2O3\ 5\,
                                                                 HCl to pH 2 \9\.
    3, 4. Acrolein and acrylonitrile.  G, FP-lined septum.....  Cool, <=6 [deg]C \18\,   14 days.\10\
                                                                 0.008% Na2S2O3, pH to
                                                                 4-5\10\.
    23, 30, 44, 49, 53, 77, 80, 81,    G, FP-lined cap........  Cool, <=6 [deg]C \18\,   7 days until
     98, 100, 112. Phenols \11\.                                 0.008% Na2S2O3.          extraction, 40 days
                                                                                          after extraction.
    7, 38. Benzidines 11,12..........  G, FP-lined cap........  Cool, <=6 [deg]C \18\,   7 days until
                                                                 0.008% Na2S2O3\5\.       extraction.\13\
    14, 17, 48, 50-52. Phthalate       G, FP-lined cap........  Cool, <=6 [deg]C \18\..  7 days until
     esters \11\.                                                                         extraction, 40 days
                                                                                          after extraction.
    82-84. Nitrosamines 11,14........  G, FP-lined cap........  Cool, <=6 [deg]C\18\,    7 days until
                                                                 store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3\5\.              after extraction.
    88-94. PCBs \11\.................  G, FP-lined cap........  Cool, <=6 [deg]C \18\..  1 year until
                                                                                          extraction, 1 year
                                                                                          after extraction.
    54, 55, 75, 79. Nitroaromatics     G, FP-lined cap........  Cool, <=6 [deg]C \18\,   7 days until
     and isophorone \11\.                                        store in dark, 0.008%    extraction, 40 days
                                                                 Na2S2O3\5\.              after extraction.
    1, 2, 5, 8-12, 32, 33, 58, 59,     G, FP-lined cap........  Cool, <=6 [deg]C \18\,   7 days until
     74, 78, 99, 101. Polynuclear                                store in dark, 0.008%    extraction, 40 days
     aromatic hydrocarbons \11\.                                 Na2S2O3\5\.              after extraction.
    15, 16, 21, 31, 87. Haloethers     G, FP-lined cap........  Cool, <=6 [deg]C \18\,   7 days until
     \11\.                                                       0.008% Na2S2O3\5\.       extraction, 40 days
                                                                                          after extraction.
    29, 35-37, 63-65, 107.             G, FP-lined cap........  Cool, <=6 [deg]C \18\..  7 days until
     Chlorinated hydrocarbons \11\.                                                       extraction, 40 days
                                                                                          after extraction.
    60-62, 66-72, 85, 86, 95-97, 102,  .......................
     103. CDDs/CDFs \11\.
    Aqueous Samples: Field and Lab     G......................  Cool, <=6 [deg]C \18\,   1 year.
     Preservation.                                               0.008% Na2S2O3\5\, pH
                                                                 <9.
    Solids and Mixed-Phase Samples:    G......................  Cool, <=6 [deg]C \18\..  7 days.
     Field Preservation.
    Tissue Samples: Field              G......................  Cool, <=6 [deg]C \18\..  24 hours.
     Preservation.
    Solids, Mixed-Phase, and Tissue    G......................  Freeze, <= -10 [deg]C..  1 year.
     Samples: Lab Preservation.
    114-118. Alkylated phenols.......  G......................  Cool, <6 [deg]C, H2SO4   28 days until
                                                                 to pH <2.                extraction, 40 days
                                                                                          after extraction.
    119. Adsorbable Organic Halides    G......................  Cool, <6 [deg]C, 0.008%  Hold at least 3 days,
     (AOX).                                                      Na2S2O3 HNO3 to pH <2.   but not more than 6
                                                                                          months.
    120. Chlorinated Phenolics.......  .......................  Cool, <6 [deg]C, 0.008%  30 days until
                                                                 Na2S2O3 H2SO4 to pH <2.  acetylation, 30 days
                                                                                          after acetylation.
Table ID--Pesticides Tests:
    1-70. Pesticides \11\............  G, FP-lined cap........  Cool, <=6 [deg]C\18\,    7 days until
                                                                 pH 5-9-\15\.             extraction, 40 days
                                                                                          after extraction.
Table IE--Radiological Tests:
    1-5. Alpha, beta, and radium.....  P, FP, G...............  HNO3 to pH <2..........  6 months.
Table IH--Bacterial Tests:
    1. E. coli.......................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.0008% Na2S2O3\5\.
    2. Enterococci...................  PA, G..................  Cool, <10 [deg]C,        8 hours.\22\
                                                                 0.0008% Na2S2O3\ 5\.
Table IH--Protozoan Tests:             .......................
    8. Cryptosporidium...............  LDPE; field filtration.  1-10 [deg]C............  96 hours.\21\
    9. Giardia.......................  LDPE; field filtration.  1-10 [deg]C............  96 hours.\21\
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is for polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE); Teflon[supreg]), or
  other fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is
  made of a sterilizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density
  polyethylene.

[[Page 29808]]

 
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
  minutes of collection. For a composite sample collected with an automated sample (e.g., using a 24-hour
  composite sample; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at <= 6
  [deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
  sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <= 6
  [deg]C, unless specified otherwise in this Table II or in the method(s), until collection, splitting, and
  preservation is completed. Add the preservative to the sample container prior to sample collection when the
  preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a
  composite sample within 15 minutes of collection. If a composite measurement is required but a composite
  sample would compromise sample integrity, individual grab samples must be collected at prescribed time
  intervals (e.g., 4 samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed
  separately and the concentrations averaged. Alternatively, grab samples may be collected in the field and
  composited in the laboratory if the compositing procedure produces results equivalent to results produced by
  arithmetic averaging of results of analysis of individual grab samples. For examples of laboratory compositing
  procedures, see EPA Method 1664 Rev. A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and (v)
  (volatile organics).
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
  the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering such
  material for transportation is responsible for ensuring such compliance. For the preservation requirement of
  Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
  determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
  (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater; Nitric acid
  (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
  acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
  Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
  less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
  samples may be held before the start of analysis and still be considered valid. Samples may be held for longer
  periods only if the permittee or monitoring laboratory has data on file to show that, for the specific types
  of samples under study, the analytes are stable for the longer time, and has received a variance from the
  Regional Administrator under Sec. 136.3(e). For a grab sample, the holding time begins at the time of
  collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
  sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR part 403, Appendix E), the holding time begins at the time of
  the end of collection of the composite sample. For a set of grab samples composited in the field or
  laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
  may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
  obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
  sample stability. See 136.3(e) for details. The date and time of collection of an individual grab sample is
  the date and time at which the sample is collected. For a set of grab samples to be composited, and that are
  all collected on the same calendar date, the date of collection is the date on which the samples are
  collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
  date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
  automatically on a given date, the date of collection is the date on which the sample is collected. For a
  composite sample collected automatically, and that is collected across two calendar dates, the date of
  collection is the dates of the two days; e.g., November 14-15. For static-renewal toxicity tests, each grab or
  composite sample may also be used to prepare test solutions for renewal at 24 h, 48 h, and/or 72 h after first
  use, if stored at 0-6 [deg]C, with minimum head space.
\5\ ASTM D7365-09a specifies treatment options for samples containing oxidants (e.g., chlorine). Also, Section
  9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses
  dechlorination procedures.
\6\ Sampling, preservation and mitigating interferences in water samples for analysis of cyanide are described
  in ASTM D7365-09a. There may be interferences that are not mitigated by the analytical test methods or D7365-
  09a. Any technique for removal or suppression of interference may be employed, provided the laboratory
  demonstrates that it more accurately measures cyanide through quality control measures described in the
  analytical test method. Any removal or suppression technique not described in D7365-09a or the analytical test
  method must be documented along with supporting data.
\7\ For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives.
  For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40
  CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of
  collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will
  be compromised during collection of a composite sample collected automatically over time (e.g., by interchange
  of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote
  2) in place of a composite sample collected automatically.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
\10\ The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
  adjustment must be analyzed within 3 days of sampling.
\11\ When the extractable analytes of concern fall within a single chemical category, the specified preservative
  and maximum holding times should be observed for optimum safeguard of sample integrity (i.e., use all
  necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two
  or more chemical categories, the sample may be preserved by cooling to <= 6 [deg]C, reducing residual chlorine
  with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this
  manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this
  optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
  thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
\12\ If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0  0.2 to
  prevent rearrangement to benzidine.
\13\ Extracts may be stored up to 30 days at < 0 [deg]C.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
  of sampling.
\15\ The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
  extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Place sufficient ice with the samples in the shipping container to ensure that ice is still present when
  the samples arrive at the laboratory. However, even if ice is present when the samples arrive, immediately
  measure the temperature of the samples and confirm that the preservation temperature maximum has not been
  exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the
  permittee can be given the option of on-site testing or can request a variance. The request for a variance
  should include supportive data which show that the toxicity of the effluent samples is not reduced because of
  the increased holding temperature. Aqueous samples must not be frozen. Hand-delivered samples used on the day
  of collection do not need to be cooled to 0 to 6 [deg]C prior to test initiation.
\17\ Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be
  collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48
  hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
  sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory
  within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample
  should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669.
  If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be
  filtered in a designated clean area in the field within the time period necessary to maintain sample
  integrity. A sample that has been collected for determination of total or dissolved trace level mercury must
  be analyzed within 90 days of sample collection.
\18\ Aqueous samples must be preserved at <= 6 [deg]C, and should not be frozen unless data demonstrating that
  sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
  regulatory authority. Also, for purposes of NPDES monitoring, the specification of ``<= [deg]C'' is used in
  place of the ``4 [deg]C'' and ``< 4 [deg]C'' sample temperature requirements listed in some methods. It is not
  necessary to measure the sample temperature to three significant figures (1/100th of 1 degree); rather, three
  significant figures are specified so that rounding down to 6 [deg]C may not be used to meet the <=6 [deg]C
  requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than
  15 minutes).

[[Page 29809]]

 
\19\ An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at
  least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must
  be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment
  samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and
  holding time requirements in the approved metals methods.
\20\ To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6.
  The allowance in this footnote supersedes preservation and holding time requirements in the approved
  hexavalent chromium methods, unless this supersession would compromise the measurement, in which case
  requirements in the method must be followed.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
  in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
\22\ Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later
  than 8 hours from time of collection.
\23\ For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for
  the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B
  aerobically digested, and Class B anaerobically digested.
\24\ The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-
  available form of orthophosphorus (i.e., that which passes through a 0.45-micron filter), hence the
  requirement to filter the sample immediately upon collection (i.e., within 15 minutes of collection).


0
4. Section 136.4 is revised to read as follows:


Sec.  136.4  Application for and approval of alternate test procedures 
for nationwide use.

    (a) A written application for review of an alternate test procedure 
(alternate method) for nationwide use may be made by letter via email 
or by hard copy in triplicate to the National Alternate Test Procedure 
(ATP) Program Coordinator (National Coordinator), Office of Science and 
Technology (4303T), Office of Water, U.S. Environmental Protection 
Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460. Any 
application for an alternate test procedure (ATP) under this paragraph 
(a) shall:
    (1) Provide the name and address of the responsible person or firm 
making the application.
    (2) Identify the pollutant(s) or parameter(s) for which nationwide 
approval of an alternate test procedure is being requested.
    (3) Provide a detailed description of the proposed alternate test 
procedure, together with references to published or other studies 
confirming the general applicability of the alternate test procedure 
for the analysis of the pollutant(s) or parameter(s) in wastewater 
discharges from representative and specified industrial or other 
categories.
    (4) Provide comparability data for the performance of the proposed 
alternative test procedure compared to the performance of the reference 
method.
    (b) The National Coordinator may request additional information and 
analyses from the applicant in order to determine whether the alternate 
test procedure satisfies the applicable requirements of this Part.
    (c) Approval for nationwide use. (1) After a review of the 
application and any additional analyses requested from the applicant, 
the National Coordinator will notify the applicant, in writing, of 
acceptance or rejection of the alternate test procedure for nationwide 
use in CWA programs. If the application is not approved, the National 
Coordinator will specify what additional information might lead to a 
reconsideration of the application, and notify the Regional Alternate 
Test Procedure Coordinators of such rejection. Based on the National 
Coordinator's rejection of a proposed alternate test procedure and an 
assessment of any approvals for limited uses for the unapproved method, 
the Regional ATP Coordinator or permitting authority may decide to 
withdraw approval of the method for limited use in the Region.
    (2) Where the National Coordinator approved an applicant's request 
for nationwide use of an alternate test procedure, the National 
Coordinator will notify the applicant that the National Coordinator 
will recommend rulemaking to approve the alternate test procedure. The 
National Coordinator will notify the Regional ATP Coordinator or 
permitting authorities that they may consider approval of this 
alternate test procedure for limited use in their Regions based on the 
information and data provided in the applicant's application. The 
Regional ATP Coordinator or permitting authority will grant approval on 
a case-by-case basis prior to use of the alternate test procedure for 
compliance analyses until the alternate test procedure is approved by 
publication in a final rule in the Federal Register.
    (3) EPA will propose to amend 40 CFR Part 136 to include the 
alternate test procedure in Sec.  136.3. EPA shall make available for 
review all the factual bases for its proposal, including any 
performance data submitted by the applicant and any available EPA 
analysis of those data.
    (4) Following public comment, EPA shall publish in the Federal 
Register a final decision on whether to amend 40 CFR Part 136 to 
include the alternate test procedure as an approved analytical method.
    (5) Whenever the National Coordinator has approved an applicant's 
request for nationwide use of an alternate test procedure, any person 
may request an approval of the method for limited use under Sec.  136.5 
from the EPA Region.

0
5. Section 136.5 is revised to read as follows:


Sec.  136.5  Approval of alternate test procedures for limited use.

    (a) Any person may request the Regional Alternate Test Procedure 
(ATP) Coordinator or permitting authority to approve the use of an 
alternate test procedure in the Region.
    (b) When the request for the use of an alternate test procedure 
concerns use in a State with an NPDES permit program approved pursuant 
to section 402 of the Act, the requestor shall first submit an 
application for limited use to the Director of the State agency having 
responsibility for issuance of NPDES permits within such State (i.e., 
permitting authority). The Director will forward the application to the 
Regional ATP Coordinator or permitting authority with a recommendation 
for or against approval.
    (c) Any application for approval of an alternate test procedure for 
limited use may be made by letter, email or by hard copy. The 
application shall include the following:
    (1) Provide the name and address of the applicant and the 
applicable ID number of the existing or pending permit and issuing 
agency for which use of the alternate test procedure is requested, and 
the discharge serial number.
    (2) Identify the pollutant or parameter for which approval of an 
alternate test procedure is being requested.
    (3) Provide justification for using testing procedures other than 
those specified in Tables IA through IH of Sec.  136.3, or in the NPDES 
permit.
    (4) Provide a detailed description of the proposed alternate test 
procedure, together with references to published studies of the 
applicability of the alternate test procedure to the effluents in 
question.

[[Page 29810]]

    (5) Provide comparability data for the performance of the proposed 
alternate test procedure compared to the performance of the reference 
method.
    (d) Approval for limited use. (1) After a review of the application 
by the Alternate Test Procedure Regional ATP Coordinator or permitting 
authority, the Regional ATP Coordinator or permitting authority 
notifies the applicant and the appropriate State agency of approval or 
rejection of the use of the alternate test procedure. The approval may 
be restricted to use only with respect to a specific discharge or 
facility (and its laboratory) or, at the discretion of the Regional ATP 
Coordinator or permitting authority, to all discharger or facilities 
(and their associated laboratories) specified in the approval for the 
Region. If the application is not approved, the Regional ATP 
Coordinator or permitting authority shall specify what additional 
information might lead to a reconsideration of the application.
    (2) The Regional ATP Coordinator or permitting authority will 
forward a copy of every approval and rejection notification to the 
National Alternate Test Procedure Coordinator.

0
6. Section 136.6 is revised to read as follows:


Sec.  136.6  Method modifications and analytical requirements.

    (a) Definitions of terms used in this section--(1) Analyst means 
the person or laboratory using a test procedure (analytical method) in 
this Part.
    (2) Chemistry of the method means the reagents and reactions used 
in a test procedure that allow determination of the analyte(s) of 
interest in an environmental sample.
    (3) Determinative technique means the way in which an analyte is 
identified and quantified (e.g., colorimetry, mass spectrometry).
    (4) Equivalent performance means that the modified method produces 
results that meet or exceed the QC acceptance criteria of the approved 
method.
    (5) Method-defined analyte means an analyte defined solely by the 
method used to determine the analyte. Such an analyte may be a physical 
parameter, a parameter that is not a specific chemical, or a parameter 
that may be comprised of a number of substances. Examples of such 
analytes include temperature, oil and grease, total suspended solids, 
total phenolics, turbidity, chemical oxygen demand, and biochemical 
oxygen demand.
    (6) QC means ``quality control.''
    (b) Method modifications. (1) If the underlying chemistry and 
determinative technique in a modified method are essentially the same 
as an approved Part 136 method, then the modified method is an 
equivalent and acceptable alternative to the approved method provided 
the requirements of this section are met. However, those who develop or 
use a modification to an approved (Part 136) method must document that 
the performance of the modified method, in the matrix to which the 
modified method will be applied, is equivalent to the performance of 
the approved method. If such a demonstration cannot be made and 
documented, then the modified method is not an acceptable alternative 
to the approved method. Supporting documentation must, if applicable, 
include the routine initial demonstration of capability and ongoing QC 
including determination of precision and accuracy, detection limits, 
and matrix spike recoveries. Initial demonstration of capability 
typically includes analysis of four replicates of a mid-level standard 
and a method detection limit study. Ongoing quality control typically 
includes method blanks, mid-level laboratory control samples, and 
matrix spikes (QC is as specified in the method). The method is 
considered equivalent if the quality control requirements in the 
reference method are achieved. The method user's Standard Operating 
Procedure (SOP) must clearly document the modifications made to the 
reference method. Examples of allowed method modifications are listed 
in this section. The user must notify their permitting authority of the 
intent to use a modified method. Such notification should be of the 
form ``Method xxx has been modified within the flexibility allowed in 
40 CFR 136.6.'' The user may indicate the specific paragraph of Sec.  
136.6 allowing the method modification. However, specific details of 
the modification need not be provided, but must be documented in the 
Standard Operating Procedure (SOP). If the method user is uncertain 
whether a method modification is allowed, the Regional ATP Coordinator 
or permitting authority should be contacted for approval prior to 
implementing the modification. The method user should also complete 
necessary performance checks to verify that acceptable performance is 
achieved with the method modification prior to analyses of compliance 
samples.
    (2) Requirements. The modified method must be sufficiently 
sensitive and meet or exceed performance of the approved method(s) for 
the analyte(s) of interest, as documented by meeting the initial and 
ongoing quality control requirements in the method.
    (i) Requirements for establishing equivalent performance. If the 
approved method contains QC tests and QC acceptance criteria, the 
modified method must use these QC tests and the modified method must 
meet the QC acceptance criteria with the following conditions:
    (A) The analyst may only rely on QC tests and QC acceptance 
criteria in a method if it includes wastewater matrix QC tests and QC 
acceptance criteria (e.g., matrix spikes) and both initial (start-up) 
and ongoing QC tests and QC acceptance criteria.
    (B) If the approved method does not contain QC tests and QC 
acceptance criteria or if the QC tests and QC acceptance criteria in 
the method do not meet the requirements of this section, then the 
analyst must employ QC tests published in the ``equivalent'' of a Part 
136 method that has such QC, or the essential QC requirements specified 
at 136.7, as applicable. If the approved method is from a compendium or 
VCSB and the QA/QC requirements are published in other parts of that 
organization's compendium rather than within the Part 136 method then 
that part of the organization's compendium must be used for the QC 
tests.
    (C) In addition, the analyst must perform ongoing QC tests, 
including assessment of performance of the modified method on the 
sample matrix (e.g., analysis of a matrix spike/matrix spike duplicate 
pair for every twenty samples), and analysis of an ongoing precision 
and recovery sample (e.g., laboratory fortified blank or blank spike) 
and a blank with each batch of 20 or fewer samples.
    (D) If the performance of the modified method in the wastewater 
matrix or reagent water does not meet or exceed the QC acceptance 
criteria, the method modification may not be used.
    (ii) Requirements for documentation. The modified method must be 
documented in a method write-up or an addendum that describes the 
modification(s) to the approved method prior to the use of the method 
for compliance purposes. The write-up or addendum must include a 
reference number (e.g., method number), revision number, and revision 
date so that it may be referenced accurately. In addition, the 
organization that uses the modified method must document the results of 
QC tests and keep these records, along with a copy of the method write-
up or addendum, for review by an auditor.
    (3) Restrictions. An analyst may not modify an approved Clean Water 
Act analytical method for a method-defined

[[Page 29811]]

analyte. In addition, an analyst may not modify an approved method if 
the modification would result in measurement of a different form or 
species of an analyte. Changes in method procedures are not allowed if 
such changes would alter the defined chemistry (i.e., method principle) 
of the unmodified method. For example, phenol method 420.1 or 420.4 
defines phenolics as ferric iron oxidized compounds that react with 4-
aminoantipyrine (4-AAP) at pH 10 after being distilled from acid 
solution. Because total phenolics represents a group of compounds that 
all react at different efficiencies with 4-AAP, changing test 
conditions likely would change the behavior of these different phenolic 
compounds. An analyst may not modify any sample collection, 
preservation, or holding time requirements of an approved method. Such 
modifications to sample collection, preservation, and holding time 
requirements do not fall within the scope of the flexibility allowed at 
Sec.  136.6. Method flexibility refers to modifications of the 
analytical procedures used for identification and measurement of the 
analyte only and does not apply to sample collection, preservation, or 
holding time procedures, which may only be modified as specified in 
Sec.  136.3(e).
    (4) Allowable changes. Except as noted under paragraph (b)(3) of 
this section, an analyst may modify an approved test procedure 
(analytical method) provided that the underlying reactions and 
principles used in the approved method remain essentially the same, and 
provided that the requirements of this section are met. If equal or 
better performance can be obtained with an alternative reagent, then it 
is allowed. A laboratory wishing to use these modifications must 
demonstrate acceptable method performance by performing and documenting 
all applicable initial demonstration of capability and ongoing QC tests 
and meeting all applicable QC acceptance criteria as described in Sec.  
136.7. Some examples of the allowed types of changes, provided the 
requirements of this section are met include:
    (i) Changes between manual method, flow analyzer, and discrete 
instrumentation.
    (ii) Changes in chromatographic columns or temperature programs.
    (iii) Changes between automated and manual sample preparation, such 
as digestions, distillations, and extractions; in-line sample 
preparation is an acceptable form of automated sample preparation for 
CWA methods.
    (iv) In general, ICP-MS is a sensitive and selective detector for 
metal analysis; however isobaric interference can cause problems for 
quantitative determination, as well as identification based on the 
isotope pattern. Interference reduction technologies, such as collision 
cells or reaction cells, are designed to reduce the effect of 
spectroscopic interferences that may bias results for the element of 
interest. The use of interference reduction technologies is allowed, 
provided the method performance specifications relevant to ICP-MS 
measurements are met.
    (v) The use of EPA Method 200.2 or the sample preparation steps 
from EPA Method 1638, including the use of closed-vessel digestion, is 
allowed for EPA Method 200.8, provided the method performance 
specifications relevant to the ICP-MS are met.
    (vi) Changes in pH adjustment reagents. Changes in compounds used 
to adjust pH are acceptable as long as they do not produce 
interference. For example, using a different acid to adjust pH in 
colorimetric methods.
    (vii) Changes in buffer reagents are acceptable provided that the 
changes do not produce interferences.
    (viii) Changes in the order of reagent addition are acceptable 
provided that the change does not alter the chemistry and does not 
produce an interference. For example, using the same reagents, but 
adding them in different order, or preparing them in combined or 
separate solutions (so they can be added separately), is allowed, 
provided reagent stability or method performance is equivalent or 
improved.
    (ix) Changes in calibration range (provided that the modified range 
covers any relevant regulatory limit and the method performance 
specifications for calibration are met).
    (x) Changes in calibration model. (A) Linear calibration models do 
not adequately fit calibration data with one or two inflection points. 
For example, vendor-supplied data acquisition and processing software 
on some instruments may provide quadratic fitting functions to handle 
such situations. If the calibration data for a particular analytical 
method routinely display quadratic character, using quadratic fitting 
functions may be acceptable. In such cases, the minimum number of 
calibrators for second order fits should be six, and in no case should 
concentrations be extrapolated for instrument responses that exceed 
that of the most concentrated calibrator. Examples of methods with 
nonlinear calibration functions include chloride by SM4500-Cl-E-1997, 
hardness by EPA Method 130.1, cyanide by ASTM D6888 or OIA1677, 
Kjeldahl nitrogen by PAI-DK03, and anions by EPA Method 300.0.
    (B) As an alternative to using the average response factor, the 
quality of the calibration may be evaluated using the Relative Standard 
Error (RSE). The acceptance criterion for the RSE is the same as the 
acceptance criterion for Relative Standard Deviation (RSD), in the 
method. RSE is calculated as:
[GRAPHIC] [TIFF OMITTED] TR18MY12.000

Where:

x'i = Calculated concentration at level i
xi = Actual concentration of the calibration level i
n = Number of calibration points
p = Number of terms in the fitting equation (average = 1, linear = 
2, quadratic = 3)

    (C) Using the RSE as a metric has the added advantage of allowing 
the same numerical standard to be applied to the calibration model, 
regardless of the form of the model. Thus, if a method states that the 
RSD should be <=20% for the traditional linear model through the 
origin, then the RSE acceptance limit can remain <=20% as well. 
Similarly, if a method provides an RSD acceptance limit of <=15%, then 
that same figure can be used as the acceptance limit for the RSE. The 
RSE may be used as an alternative to correlation coefficients and 
coefficients of determination for evaluating calibration curves for any 
of

[[Page 29812]]

the methods at Part 136. If the method includes a numerical criterion 
for the RSD, then the same numerical value is used for the RSE. Some 
older methods do not include any criterion for the calibration curve--
for these methods, if RSE is used the value should be <=20%. Note that 
the use of the RSE is included as an alternative to the use of the 
correlation coefficient as a measure of the suitability of a 
calibration curve. It is not necessary to evaluate both the RSE and the 
correlation coefficient.
    (xi) Changes in equipment such as equipment from a vendor different 
from the one specified in the method.
    (xii) The use of micro or midi distillation apparatus in place of 
macro distillation apparatus.
    (xiii) The use of prepackaged reagents.
    (xiv) The use of digital titrators and methods where the underlying 
chemistry used for the determination is similar to that used in the 
approved method.
    (xv) Use of selected ion monitoring (SIM) mode for analytes that 
cannot be effectively analyzed in full-scan mode and reach the required 
sensitivity. False positives are more of a concern when using SIM 
analysis, so at a minimum, one quantitation and two qualifying ions 
must be monitored for each analyte (unless fewer than three ions with 
intensity greater than 15% of the base peak are available). The ratio 
of each of the two qualifying ions to the quantitation ion must be 
evaluated and should agree with the ratio observed in an authentic 
standard within 20 percent. Analyst judgment must be 
applied to the evaluation of ion ratios because the ratios can be 
affected by co-eluting compounds present in the sample matrix. The 
signal-to-noise ratio of the least sensitive ion should be at least 
3:1. Retention time in the sample should match within 0.05 minute of an 
authentic standard analyzed under identical conditions. Matrix 
interferences can cause minor shifts in retention time and may be 
evident as shifts in the retention times of the internal standards. The 
total scan time should be such that a minimum of eight scans are 
obtained per chromatographic peak.
    (xvi) Changes are allowed in purge-and-trap sample volumes or 
operating conditions. Some examples are:
    (A) Changes in purge time and purge-gas flow rate. A change in 
purge time and purge-gas flow rate is allowed provided that sufficient 
total purge volume is used to achieve the required minimum detectible 
concentration and calibration range for all compounds. In general, a 
purge rate in the range 20-200 mL/min and a total purge volume in the 
range 240-880 mL are recommended.
    (B) Use of nitrogen or helium as a purge gas, provided that the 
required sensitivities for all compounds are met.
    (C) Sample temperature during the purge state. Gentle heating of 
the sample during purging (e.g., 40 [deg]C) increases purging 
efficiency of hydrophilic compounds and may improve sample-to-sample 
repeatability because all samples are purged under precisely the same 
conditions.
    (D) Trap sorbent. Any trap design is acceptable, provided that the 
data acquired meet all QC criteria.
    (E) Changes to the desorb time. Shortening the desorb time (e.g., 
from 4 minutes to 1 minute) may not affect compound recoveries, and can 
shorten overall cycle time and significantly reduce the amount of water 
introduced to the analytical system, thus improving the precision of 
analysis, especially for water-soluble analytes. A desorb time of four 
minutes is recommended, however a shorter desorb time may be used, 
provided that all QC specifications in the method are met.
    (F) Use of water management techniques is allowed. Water is always 
collected on the trap along with the analytes and is a significant 
interference for analytical systems (GC and GC/MS). Modern water 
management techniques (e.g., dry purge or condensation points) can 
remove moisture from the sample stream and improve analytical 
performance.
    (xvii) The following modifications are allowable when performing 
EPA Method 625: The base/neutral and acid fractions may be added 
together and analyzed as one extract, provided that the analytes can be 
reliably identified and quantified in the combined extracts; the pH 
extraction sequence may be reversed to better separate acid and neutral 
components; neutral components may be extracted with either acid or 
base components; a smaller sample volume may be used to minimize matrix 
interferences provided matrix interferences are demonstrated and 
documented; alternative surrogate and internal standard concentrations 
other than those specified in the method are acceptable, provided that 
method performance is not degraded; an alternative concentration range 
may be used for the calibration other than the range specified in the 
method; the solvent for the calibration standards may be changed to 
match the solvent of the final sample extract.
    (xviii) If the characteristics of a wastewater matrix prevent 
efficient recovery of organic pollutants and prevent the method from 
meeting QC requirements, the analyst may attempt to resolve the issue 
by adding salts to the sample, provided that such salts do not react 
with or introduce the target pollutant into the sample (as evidenced by 
the analysis of method blanks, laboratory control samples, and spiked 
samples that also contain such salts), and that all requirements of 
paragraph (b)(2) of this section are met. Samples having residual 
chlorine or other halogen must be dechlorinated prior to the addition 
of such salts.
    (xix) If the characteristics of a wastewater matrix result in poor 
sample dispersion or reagent deposition on equipment and prevent the 
analyst from meeting QC requirements, the analyst may attempt to 
resolve the issue by adding a inert surfactant that does not affect the 
chemistry of the method, such as Brij-35 or sodium dodecyl sulfate 
(SDS), provided that such surfactant does not react with or introduce 
the target pollutant into the sample (as evidenced by the analysis of 
method blanks, laboratory control samples, and spiked samples that also 
contain such surfactant) and that all requirements of paragraph (b)(1) 
and (b)(2) of this section are met. Samples having residual chlorine or 
other halogen must be dechlorinated prior to the addition of such 
surfactant.
    (xx) The use of gas diffusion (using pH change to convert the 
analyte to gaseous form and/or heat to separate an analyte contained in 
steam from the sample matrix) across a hydrophobic semi-permeable 
membrane to separate the analyte of interest from the sample matrix may 
be used in place of manual or automated distillation in methods for 
analysis such as ammonia, total cyanide, total Kjeldahl nitrogen, and 
total phenols. These procedures do not replace the digestion procedures 
specified in the approved methods and must be used in conjunction with 
those procedures.
    (xxi) Changes in equipment operating parameters such as the 
monitoring wavelength of a colorimeter or the reaction time and 
temperature as needed to achieve the chemical reactions defined in the 
unmodified CWA method. For example, molybdenum blue phosphate methods 
have two absorbance maxima, one at about 660 nm and another at about 
880 nm. The former is about 2.5 times less sensitive than the latter. 
Wavelength choice provides a cost-effective, dilution-free means to 
increase sensitivity of molybdenum blue phosphate methods.
    (xxii) Interchange of oxidants, such as the use of titanium oxide 
in UV-assisted automated digestion of TOC and total

[[Page 29813]]

phosphorus, as long as complete oxidation can be demonstrated.
    (xxii) Use of an axially viewed torch with Method 200.7.
0
7. Add new Sec.  136.7 to read as follows:


Sec.  136.7  Quality assurance and quality control.

    The permittee/laboratory shall use suitable QA/QC procedures when 
conducting compliance analyses with any Part 136 chemical method or an 
alternative method specified by the permitting authority. These QA/QC 
procedures are generally included in the analytical method or may be 
part of the methods compendium for approved Part 136 methods from a 
consensus organization. For example, Standard Methods contains QA/QC 
procedures in the Part 1000 section of the Standard Methods Compendium. 
The permittee/laboratory shall follow these QA/QC procedures, as 
described in the method or methods compendium. If the method lacks QA/
QC procedures, the permittee/laboratory has the following options to 
comply with the QA/QC requirements:
    (a) Refer to and follow the QA/QC published in the ``equivalent'' 
EPA method for that parameter that has such QA/QC procedures;
    (b) Refer to the appropriate QA/QC section(s) of an approved Part 
136 method from a consensus organization compendium;
    (c)(1) Incorporate the following twelve quality control elements, 
where applicable, into the laboratory's documented standard operating 
procedure (SOP) for performing compliance analyses when using an 
approved Part 136 method when the method lacks such QA/QC procedures. 
One or more of the twelve QC elements may not apply to a given method 
and may be omitted if a written rationale is provided indicating why 
the element(s) is/are inappropriate for a specific method.
    (i) Demonstration of Capability (DOC);
    (ii) Method Detection Limit (MDL);
    (iii) Laboratory reagent blank (LRB), also referred to as method 
blank (MB);
    (iv) Laboratory fortified blank (LFB), also referred to as a spiked 
blank, or laboratory control sample (LCS);
    (v) Matrix spike (MS) and matrix spike duplicate (MSD), or 
laboratory fortified matrix (LFM) and LFM duplicate, may be used for 
suspected matrix interference problems to assess precision;
    (vi) Internal standards (for GC/MS analyses), surrogate standards 
(for organic analysis) or tracers (for radiochemistry);
    (vii) Calibration (initial and continuing), also referred to as 
initial calibration verification (ICV) and continuing calibration 
verification (CCV);
    (viii) Control charts (or other trend analyses of quality control 
results);
    (ix) Corrective action (root cause analysis);
    (x) QC acceptance criteria;
    (xi) Definitions of preparation and analytical batches that may 
drive QC frequencies; and
    (xii) Minimum frequency for conducting all QC elements.
    (2) These twelve quality control elements must be clearly 
documented in the written standard operating procedure for each 
analytical method not containing QA/QC procedures, where applicable.

0
8. Revise Appendix C to Part 136 to read as follows.

APPENDIX C TO PART 136--DETERMINATION OF METALS AND TRACE ELEMENTS IN 
WATER AND WASTES BY INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION 
SPECTROMETRY METHOD 200.7

1.0 Scope and Application

    1.1 Inductively coupled plasma-atomic emission spectrometry 
(ICP-AES) is used to determine metals and some nonmetals in 
solution. This method is a consolidation of existing methods for 
water, wastewater, and solid wastes.1-4 (For analysis of 
petroleum products see References 5 and 6, Section 16.0). This 
method is applicable to the following analytes:

------------------------------------------------------------------------
                                                      Chemical abstract
                      Analyte                         services registry
                                                       number (CASRN)
------------------------------------------------------------------------
Aluminum (Al).....................................             7429-90-5
Antimony (Sb).....................................             7440-36-0
Arsenic (As)......................................             7440-38-2
Barium (Ba).......................................             7440-39-3
Beryllium (Be)....................................             7440-41-7
Boron (B).........................................             7440-42-8
Cadmium (Cd)......................................             7440-43-9
Calcium (Ca)......................................             7440-70-2
Cerium \a\ (Cr)...................................             7440-45-1
Chromium (Cr).....................................             7440-47-3
Cobalt (Co).......................................             7440-48-4
Copper (Cu).......................................             7440-50-8
Iron (Fe).........................................             7439-89-6
Lead (Pb).........................................             7439-92-1
Lithium (Li)......................................             7439-93-2
Magnesium (Mg)....................................             7439-95-4
Manganese (Mn)....................................             7439-96-5
Mercury (Hg)......................................             7439-97-6
Molybdenum (Mo)...................................             7439-98-7
Nickel (Ni).......................................             7440-02-0
Phosphorus (P)....................................             7723-14-0
Potassium (K).....................................             7440-09-7
Selenium (Se).....................................             7782-49-2
Silica \b\ (Si02).................................             7631-86-9
Silver (Ag).......................................             7440-22-4
Sodium (Na).......................................             7440-23-5
Strontium (Sr)....................................             7440-24-6
Thallium (Tl).....................................             7440-28-0
Tin (Sn)..........................................             7440-31-5
Titanium (Ti).....................................             7440-32-6
Vanadium (V)......................................             7440-62-2
Zinc (Zn).........................................             7440-66-6
------------------------------------------------------------------------
\a\ Cerium has been included as method analyte for correction of
  potential interelement spectral interference.
\b\ This method is not suitable for the determination of silica in
  solids.

    1.2 For reference where this method is approved for use in 
compliance monitoring programs [e.g., Clean Water Act (NPDES) or 
Safe Drinking Water Act (SDWA)] consult both the appropriate 
sections of the Code of Federal Regulation (40 CFR Part 136 Table 1B 
for NPDES, and Part 141 Sec.  141.23 for drinking water), and the 
latest Federal Register announcements.
    1.3 ICP-AES can be used to determine dissolved analytes in 
aqueous samples after suitable filtration and acid preservation. To 
reduce potential interferences, dissolved solids should be <0.2% (w/
v) (Section 4.2).
    1.4 With the exception of silver, where this method is approved 
for the determination of certain metal and metalloid contaminants in 
drinking water, samples may be analyzed directly by pneumatic 
nebulization without acid digestion if the sample has been properly 
preserved with acid and has turbidity of <1 NTU at the time of 
analysis. This total recoverable determination procedure is referred 
to as ``direct analysis''. However, in the determination of some 
primary drinking water metal contaminants, preconcentration of the 
sample may be required prior to analysis in order to meet drinking 
water acceptance performance criteria (Sections 11.2.2 through 
11.2.7).
    1.5 For the determination of total recoverable analytes in 
aqueous and solid samples a digestion/extraction is required prior 
to analysis when the elements are not in solution (e.g., soils, 
sludges, sediments and aqueous samples that may contain particulate 
and suspended solids). Aqueous samples containing suspended or 
particulate material 1% (w/v) should be extracted as a solid type 
sample.
    1.6 When determining boron and silica in aqueous samples, only 
plastic, PTFE or quartz labware should be used from time of sample 
collection to completion of analysis. For accurate determination of 
boron in solid samples only quartz or PTFE beakers should be used 
during acid extraction with immediate transfer of an extract aliquot 
to a plastic centrifuge tube following dilution of the extract to 
volume. When possible, borosilicate glass should be avoided to 
prevent contamination of these analytes.
    1.7 Silver is only slightly soluble in the presence of chloride 
unless there is a sufficient chloride concentration to form the 
soluble chloride complex. Therefore, low recoveries of silver may 
occur in samples, fortified sample matrices and even fortified 
blanks if determined as a dissolved analyte or by ``direct 
analysis'' where the sample has not been processed using the total 
recoverable mixed acid digestion. For this reason it is recommended 
that samples be digested prior to the determination of silver.

[[Page 29814]]

The total recoverable sample digestion procedure given in this 
method is suitable for the determination of silver in aqueous 
samples containing concentrations up to 0.1 mg/L. For the analysis 
of wastewater samples containing higher concentrations of silver, 
succeeding smaller volume, well mixed aliquots should be prepared 
until the analysis solution contains <0.1 mg/L silver. The 
extraction of solid samples containing concentrations of silver >50 
mg/kg should be treated in a similar manner. Also, the extraction of 
tin from solid samples should be prepared again using aliquots <1 g 
when determined sample concentrations exceed 1%.
    1.8 The total recoverable sample digestion procedure given in 
this method will solubilize and hold in solution only minimal 
concentrations of barium in the presence of free sulfate. For the 
analysis of barium in samples having varying and unknown 
concentrations of sulfate, analysis should be completed as soon as 
possible after sample preparation.
    1.9 The total recoverable sample digestion procedure given in 
this method is not suitable for the determination of volatile 
organo-mercury compounds. However, if digestion is not required 
(turbidity <1 NTU), the combined concentrations of inorganic and 
organo-mercury in solution can be determined by ``direct analysis'' 
pneumatic nebulization provided the sample solution is adjusted to 
contain the same mixed acid (HNO3 + HCl) matrix as the 
total recoverable calibration standards and blank solutions.
    1.10 Detection limits and linear ranges for the elements will 
vary with the wavelength selected, the spectrometer, and the 
matrices. Table 1 provides estimated instrument detection limits for 
the listed wavelengths.\7\ However, actual method detection limits 
and linear working ranges will be dependent on the sample matrix, 
instrumentation, and selected operating conditions.
    1.11 Users of the method data should state the data-quality 
objectives prior to analysis. Users of the method must document and 
have on file the required initial demonstration performance data 
described in Section 9.2 prior to using the method for analysis.

2.0 Summary of Method

    2.1 An aliquot of a well mixed, homogeneous aqueous or solid 
sample is accurately weighed or measured for sample processing. For 
total recoverable analysis of a solid or an aqueous sample 
containing undissolved material, analytes are first solubilized by 
gentle refluxing with nitric and hydrochloric acids. After cooling, 
the sample is made up to volume, is mixed and centrifuged or allowed 
to settle overnight prior to analysis. For the determination of 
dissolved analytes in a filtered aqueous sample aliquot, or for the 
``direct analysis'' total recoverable determination of analytes in 
drinking water where sample turbidity is <1 NTU, the sample is made 
ready for analysis by the appropriate addition of nitric acid, and 
then diluted to a predetermined volume and mixed before analysis.
    2.2 The analysis described in this method involves 
multielemental determinations by ICP-AES using sequential or 
simultaneous instruments. The instruments measure characteristic 
atomic-line emission spectra by optical spectrometry. Samples are 
nebulized and the resulting aerosol is transported to the plasma 
torch. Element specific emission spectra are produced by a radio-
frequency inductively coupled plasma. The spectra are dispersed by a 
grating spectrometer, and the intensities of the line spectra are 
monitored at specific wavelengths by a photosensitive device. 
Photocurrents from the photosensitive device are processed and 
controlled by a computer system. A background correction technique 
is required to compensate for variable background contribution to 
the determination of the analytes. Background must be measured 
adjacent to the analyte wavelength during analysis. Various 
interferences must be considered and addressed appropriately as 
discussed in Sections 4.0, 7.0, 9.0, 10.0, and 11.0.

3.0 Definitions

    3.1 Calibration Blank--A volume of reagent water acidified with 
the same acid matrix as in the calibration standards. The 
calibration blank is a zero standard and is used to calibrate the 
ICP instrument (Section 7.10.1).
    3.2 Calibration Standard (CAL)--A solution prepared from the 
dilution of stock standard solutions. The CAL solutions are used to 
calibrate the instrument response with respect to analyte 
concentration (Section 7.9).
    3.3 Dissolved Analyte--The concentration of analyte in an 
aqueous sample that will pass through a 0.45 [mu]m membrane filter 
assembly prior to sample acidification (Section 11.1).
    3.4 Field Reagent Blank (FRB)--An aliquot of reagent water or 
other blank matrix that is placed in a sample container in the 
laboratory and treated as a sample in all respects, including 
shipment to the sampling site, exposure to the sampling site 
conditions, storage, preservation, and all analytical procedures. 
The purpose of the FRB is to determine if method analytes or other 
interferences are present in the field environment (Section 8.5).
    3.5 Instrument Detection Limit (IDL)--The concentration 
equivalent to the analyte signal which is equal to three times the 
standard deviation of a series of 10 replicate measurements of the 
calibration blank signal at the same wavelength (Table 1.).
    3.6 Instrument Performance Check (IPC) Solution--A solution of 
method analytes, used to evaluate the performance of the instrument 
system with respect to a defined set of method criteria (Sections 
7.11 and 9.3.4).
    3.7 Internal Standard--Pure analyte(s) added to a sample, 
extract, or standard solution in known amount(s) and used to measure 
the relative responses of other method analytes that are components 
of the same sample or solution. The internal standard must be an 
analyte that is not a sample component (Section 11.5).
    3.8 Laboratory Duplicates (LD1 and LD2)--Two aliquots of the 
same sample taken in the laboratory and analyzed separately with 
identical procedures. Analyses of LD1 and LD2 indicate precision 
associated with laboratory procedures, but not with sample 
collection, preservation, or storage procedures.
    3.9 Laboratory Fortified Blank (LFB)--An aliquot of LRB to which 
known quantities of the method analytes are added in the laboratory. 
The LFB is analyzed exactly like a sample, and its purpose is to 
determine whether the methodology is in control and whether the 
laboratory is capable of making accurate and precise measurements 
(Sections 7.10.3 and 9.3.2).
    3.10 Laboratory Fortified Sample Matrix (LFM)--An aliquot of an 
environmental sample to which known quantities of the method 
analytes are added in the laboratory. The LFM is analyzed exactly 
like a sample, and its purpose is to determine whether the sample 
matrix contributes bias to the analytical results. The background 
concentrations of the analytes in the sample matrix must be 
determined in a separate aliquot and the measured values in the LFM 
corrected for background concentrations (Section 9.4).
    3.11 Laboratory Reagent Blank (LRB)--An aliquot of reagent water 
or other blank matrices that are treated exactly as a sample 
including exposure to all glassware, equipment, solvents, reagents, 
and internal standards that are used with other samples. The LRB is 
used to determine if method analytes or other interferences are 
present in the laboratory environment, reagents, or apparatus 
(Sections 7.10.2 and 9.3.1).
    3.12 Linear Dynamic Range (LDR)--The concentration range over 
which the instrument response to an analyte is linear (Section 
9.2.2).
    3.13 Method Detection Limit (MDL)--The minimum concentration of 
an analyte that can be identified, measured, and reported with 99% 
confidence that the analyte concentration is greater than zero 
(Section 9.2.4 and Table 4.).
    3.14 Plasma Solution--A solution that is used to determine the 
optimum height above the work coil for viewing the plasma (Sections 
7.15 and 10.2.3).
    3.15 Quality Control Sample (QCS)--A solution of method analytes 
of known concentrations which is used to fortify an aliquot of LRB 
or sample matrix. The QCS is obtained from a source external to the 
laboratory and different from the source of calibration standards. 
It is used to check either laboratory or instrument performance 
(Sections 7.12 and 9.2.3).
    3.16 Solid Sample--For the purpose of this method, a sample 
taken from material classified as soil, sediment or sludge.
    3.17 Spectral Interference Check (SIC) Solution--A solution of 
selected method analytes of higher concentrations which is used to 
evaluate the procedural routine for correcting known interelement 
spectral interferences with respect to a defined set of method 
criteria (Sections 7.13, 7.14 and 9.3.5).
    3.18 Standard Addition--The addition of a known amount of 
analyte to the sample in order to determine the relative response of 
the detector to an analyte within the sample matrix. The relative 
response is then used to

[[Page 29815]]

assess either an operative matrix effect or the sample analyte 
concentration (Sections 9.5.1 and 11.5).
    3.19 Stock Standard Solution--A concentrated solution containing 
one or more method analytes prepared in the laboratory using assayed 
reference materials or purchased from a reputable commercial source 
(Section 7.8).
    3.20 Total Recoverable Analyte--The concentration of analyte 
determined either by ``direct analysis'' of an unfiltered acid 
preserved drinking water sample with turbidity of <1 NTU (Section 
11.2.1), or by analysis of the solution extract of a solid sample or 
an unfiltered aqueous sample following digestion by refluxing with 
hot dilute mineral acid(s) as specified in the method (Sections 11.2 
and 11.3).
    3.21 Water Sample--For the purpose of this method, a sample 
taken from one of the following sources: drinking, surface, ground, 
storm runoff, industrial or domestic wastewater.

4.0 Interferences

    4.1 Spectral interferences are caused by background emission 
from continuous or recombination phenomena, stray light from the 
line emission of high concentration elements, overlap of a spectral 
line from another element, or unresolved overlap of molecular band 
spectra.
    4.1.1 Background emission and stray light can usually be 
compensated for by subtracting the background emission determined by 
measurement(s) adjacent to the analyte wavelength peak. Spectral 
scans of samples or single element solutions in the analyte regions 
may indicate not only when alternate wavelengths are desirable 
because of severe spectral interference, but also will show whether 
the most appropriate estimate of the background emission is provided 
by an interpolation from measurements on both sides of the 
wavelength peak or by the measured emission on one side or the 
other. The location(s) selected for the measurement of background 
intensity will be determined by the complexity of the spectrum 
adjacent to the wavelength peak. The location(s) used for routine 
measurement must be free of off-line spectral interference 
(interelement or molecular) or adequately corrected to reflect the 
same change in background intensity as occurs at the wavelength 
peak.
    4.1.2 Spectral overlaps may be avoided by using an alternate 
wavelength or can be compensated for by equations that correct for 
interelement contributions, which involves measuring the interfering 
elements. Some potential on-line spectral interferences observed for 
the recommended wavelengths are given in Table 2. When operative and 
uncorrected, these interferences will produce false-positive 
determinations and be reported as analyte concentrations. The 
interferences listed are only those that occur between method 
analytes. Only interferences of a direct overlap nature that were 
observed with a single instrument having a working resolution of 
0.035 nm are listed. More extensive information on interferant 
effects at various wavelengths and resolutions is available in 
Boumans' Tables.\8\ Users may apply interelement correction factors 
determined on their instruments within tested concentration ranges 
to compensate (off-line or on-line) for the effects of interfering 
elements.
    4.1.3 When interelement corrections are applied, there is a need 
to verify their accuracy by analyzing spectral interference check 
solutions as described in Section 7.13. Interelement corrections 
will vary for the same emission line among instruments because of 
differences in resolution, as determined by the grating plus the 
entrance and exit slit widths, and by the order of dispersion. 
Interelement corrections will also vary depending upon the choice of 
background correction points. Selecting a background correction 
point where an interfering emission line may appear should be 
avoided when practical. Interelement corrections that constitute a 
major portion of an emission signal may not yield accurate data. 
Users should not forget that some samples may contain uncommon 
elements that could contribute spectral interferences.\7,8\
    4.1.4 The interference effects must be evaluated for each 
individual instrument whether configured as a sequential or 
simultaneous instrument. For each instrument, intensities will vary 
not only with optical resolution but also with operating conditions 
(such as power, viewing height and argon flow rate). When using the 
recommended wavelengths given in Table 1, the analyst is required to 
determine and document for each wavelength the effect from the known 
interferences given in Table 2, and to utilize a computer routine 
for their automatic correction on all analyses. To determine the 
appropriate location for off-line background correction, the user 
must scan the area on either side adjacent to the wavelength and 
record the apparent emission intensity from all other method 
analytes. This spectral information must be documented and kept on 
file. The location selected for background correction must be either 
free of off-line interelement spectral interference or a computer 
routine must be used for their automatic correction on all 
determinations. If a wavelength other than the recommended 
wavelength is used, the user must determine and document both the 
on-line and off-line spectral interference effect from all method 
analytes and provide for their automatic correction on all analyses. 
Tests to determine the spectral interference must be done using 
analyte concentrations that will adequately describe the 
interference. Normally, 100 mg/L single element solutions are 
sufficient, however, for analytes such as iron that may be found at 
high concentration a more appropriate test would be to use a 
concentration near the upper LDR limit. See Section 10.4 for 
required spectral interference test criteria.
    4.1.5 When interelement corrections are not used, either on-
going SIC solutions (Section 7.14) must be analyzed to verify the 
absence of interelement spectral interference or a computer software 
routine must be employed for comparing the determinative data to 
limits files for notifying the analyst when an interfering element 
is detected in the sample at a concentration that will produce 
either an apparent false positive concentration, greater than the 
analyte IDL, or false negative analyte concentration, less than the 
99% lower control limit of the calibration blank. When the 
interference accounts for 10% or more of the analyte concentration, 
either an alternate wavelength free of interference or another 
approved test procedure must be used to complete the analysis. For 
example, the copper peak at 213.853 nm could be mistaken for the 
zinc peak at 213.856 nm in solutions with high copper and low zinc 
concentrations. For this example, a spectral scan in the 213.8 nm 
region would not reveal the misidentification because a single peak 
near the zinc location would be observed. The possibility of this 
misidentification of copper for the zinc peak at 213.856 nm can be 
identified by measuring the copper at another emission line, e.g., 
324.754 nm. Users should be aware that, depending upon the 
instrumental resolution, alternate wavelengths with adequate 
sensitivity and freedom from interference may not be available for 
all matrices. In these circumstances the analyte must be determined 
using another approved test procedure.
    4.2 Physical interferences are effects associated with the 
sample nebulization and transport processes. Changes in viscosity 
and surface tension can cause significant inaccuracies, especially 
in samples containing high dissolved solids or high acid 
concentrations. If physical interferences are present, they must be 
reduced by such means as a high-solids nebulizer, diluting the 
sample, using a peristaltic pump, or using an appropriate internal 
standard element. Another problem that can occur with high dissolved 
solids is salt buildup at the tip of the nebulizer, which affects 
aerosol flow rate and causes instrumental drift. This problem can be 
controlled by a high-solids nebulizer, wetting the argon prior to 
nebulization, using a tip washer, or diluting the sample. Also, it 
has been reported that better control of the argon flow rates, 
especially for the nebulizer, improves instrument stability and 
precision; this is accomplished with the use of mass flow 
controllers.
    4.3 Chemical interferences include molecular-compound formation, 
ionization effects, and solute-vaporization effects. Normally, these 
effects are not significant with the ICP-AES technique. If observed, 
they can be minimized by careful selection of operating conditions 
(such as incident power and observation height), by buffering of the 
sample, by matrix matching, and by standard-addition procedures. 
Chemical interferences are highly dependent on matrix type and the 
specific analyte element.
    4.4 Memory interferences result when analytes in a previous 
sample contribute to the signals measured in a new sample. Memory 
effects can result from sample deposition on the uptake tubing to 
the nebulizer, and from the buildup of sample material in the plasma 
torch and spray chamber. The site where these effects occur is 
dependent on the element and can be minimized by flushing the system 
with a rinse blank between samples (Section 7.10.4). The possibility 
of memory interferences should be recognized within an analytical 
run and suitable rinse times should be used

[[Page 29816]]

to reduce them. The rinse times necessary for a particular element 
must be estimated prior to analysis. This may be achieved by 
aspirating a standard containing elements corresponding to either 
their LDR or a concentration ten times those usually encountered. 
The aspiration time should be the same as a normal sample analysis 
period, followed by analysis of the rinse blank at designated 
intervals. The length of time required to reduce analyte signals to 
within a factor of two of the method detection limit, should be 
noted. Until the required rinse time is established, this method 
requires a rinse period of at least 60 seconds between samples and 
standards. If a memory interference is suspected, the sample must be 
re-analyzed after a long rinse period.

5.0 Safety

    5.1 The toxicity or carcinogenicity of each reagent used in this 
method have not been fully established. Each chemical should be 
regarded as a potential health hazard and exposure to these 
compounds should be as low as reasonably achievable. Each laboratory 
is responsible for maintaining a current awareness file of OSHA 
regulations regarding the safe handling of the chemicals specified 
in this method.9-12 A reference file of material data 
handling sheets should also be made available to all personnel 
involved in the chemical analysis. Specifically, concentrated nitric 
and hydrochloric acids present various hazards and are moderately 
toxic and extremely irritating to skin and mucus membranes. Use 
these reagents in a fume hood whenever possible and if eye or skin 
contact occurs, flush with large volumes of water. Always wear 
safety glasses or a shield for eye protection, protective clothing 
and observe proper mixing when working with these reagents.
    5.2 The acidification of samples containing reactive materials 
may result in the release of toxic gases, such as cyanides or 
sulfides. Acidification of samples should be done in a fume hood.
    5.3 All personnel handling environmental samples known to 
contain or to have been in contact with human waste should be 
immunized against known disease causative agents.
    5.4 The inductively coupled plasma should only be viewed with 
proper eye protection from the ultraviolet emissions.
    5.5 It is the responsibility of the user of this method to 
comply with relevant disposal and waste regulations. For guidance 
see Sections 14.0 and 15.0.

6.0 Equipment and Supplies

    6.1 Inductively coupled plasma emission spectrometer:
    6.1.1 Computer-controlled emission spectrometer with background-
correction capability.

The spectrometer must be capable of meeting and complying with the 
requirements described and referenced in Section 2.2.

    6.1.2 Radio-frequency generator compliant with FCC regulations.
    6.1.3 Argon gas supply--High purity grade (99.99%). When 
analyses are conducted frequently, liquid argon is more economical 
and requires less frequent replacement of tanks than compressed 
argon in conventional cylinders.
    6.1.4 A variable speed peristaltic pump is required to deliver 
both standard and sample solutions to the nebulizer.
    6.1.5 (Optional) Mass flow controllers to regulate the argon 
flow rates, especially the aerosol transport gas, are highly 
recommended. Their use will provide more exacting control of 
reproducible plasma conditions.
    6.2 Analytical balance, with capability to measure to 0.1 mg, 
for use in weighing solids, for preparing standards, and for 
determining dissolved solids in digests or extracts.
    6.3 A temperature adjustable hot plate capable of maintaining a 
temperature of 95 [deg]C.
    6.4 (Optional) A temperature adjustable block digester capable 
of maintaining a temperature of 95 [deg]C and equipped with 250 mL 
constricted digestion tubes.
    6.5 (Optional) A steel cabinet centrifuge with guard bowl, 
electric timer and brake.
    6.6 A gravity convection drying oven with thermostatic control 
capable of maintaining 180 [deg]C  5 [deg]C.
    6.7 (Optional) An air displacement pipetter capable of 
delivering volumes ranging from 0.1-2500 [mu]L with an assortment of 
high quality disposable pipet tips.
    6.8 Mortar and pestle, ceramic or nonmetallic material.
    6.9 Polypropylene sieve, 5-mesh (4 mm opening).
    6.10 Labware--For determination of trace levels of elements, 
contamination and loss are of prime consideration. Potential 
contamination sources include improperly cleaned laboratory 
apparatus and general contamination within the laboratory 
environment from dust, etc. A clean laboratory work area designated 
for trace element sample handling must be used. Sample containers 
can introduce positive and negative errors in the determination of 
trace elements by contributing contaminants through surface 
desorption or leaching, or depleting element concentrations through 
adsorption processes. All reusable labware (glass, quartz, 
polyethylene, PTFE, FEP, etc.) should be sufficiently clean for the 
task objectives. Several procedures found to provide clean labware 
include washing with a detergent solution, rinsing with tap water, 
soaking for four hours or more in 20% (v/v) nitric acid or a mixture 
of HNO3 and HCl (1+2+9), rinsing with reagent water and 
storing clean.2 3 Chromic acid cleaning solutions must be 
avoided because chromium is an analyte.
    6.10.1 Glassware--Volumetric flasks, graduated cylinders, 
funnels and centrifuge tubes (glass and/or metal-free plastic).
    6.10.2 Assorted calibrated pipettes.
    6.10.3 Conical Phillips beakers (Corning 1080-250 or 
equivalent), 250 mL with 50 mm watch glasses.
    6.10.4 Griffin beakers, 250 mL with 75 mm watch glasses and 
(optional) 75 mm ribbed watch glasses.
    6.10.5 (Optional) PTFE and/or quartz Griffin beakers, 250 mL 
with PTFE covers.
    6.10.6 Evaporating dishes or high-form crucibles, porcelain, 100 
mL capacity.
    6.10.7 Narrow-mouth storage bottles, FEP (fluorinated ethylene 
propylene) with screw closure, 125 mL to 1 L capacities.
    6.10.8 One-piece stem FEP wash bottle with screw closure, 125 mL 
capacity.

7.0 Reagents and Standards

    7.1 Reagents may contain elemental impurities which might affect 
analytical data. Only high-purity reagents that conform to the 
American Chemical Society specifications \13\ should be used 
whenever possible. If the purity of a reagent is in question, 
analyze for contamination. All acids used for this method must be of 
ultra high-purity grade or equivalent. Suitable acids are available 
from a number of manufacturers. Redistilled acids prepared by sub-
boiling distillation are acceptable.
    7.2 Hydrochloric acid, concentrated (sp.gr. 1.19)--HCl.
    7.2.1 Hydrochloric acid (1+1)--Add 500 mL concentrated HCl to 
400 mL reagent water and dilute to 1 L.
    7.2.2 Hydrochloric acid (1+4)--Add 200 mL concentrated HCl to 
400 mL reagent water and dilute to 1 L.
    7.2.3 Hydrochloric acid (1+20)--Add 10 mL concentrated HCl to 
200 mL reagent water.
    7.3 Nitric acid, concentrated (sp.gr. 1.41)--HNO3.
    7.3.1 Nitric acid (1+1)--Add 500 mL concentrated HNO3 
to 400 mL reagent water and dilute to 1 L.
    7.3.2 Nitric acid (1+2)--Add 100 mL concentrated HNO3 
to 200 mL reagent water.
    7.3.3 Nitric acid (1+5)--Add 50 mL concentrated HNO3 
to 250 mL reagent water.
    7.3.4 Nitric acid (1+9)--Add 10 mL concentrated HNO3 
to 90 mL reagent water.
    7.4 Reagent water. All references to water in this method refer 
to ASTM Type I grade water.\14\
    7.5 Ammonium hydroxide, concentrated (sp.gr. 0.902).
    7.6 Tartaric acid, ACS reagent grade.
    7.7 Hydrogen peroxide, 50%, stabilized certified reagent grade.
    7.8 Standard Stock Solutions--Stock standards may be purchased 
or prepared from ultra-high purity grade chemicals (99.99-99.999% 
pure). All compounds must be dried for one hour at 105 [deg]C, 
unless otherwise specified. It is recommended that stock solutions 
be stored in FEP bottles. Replace stock standards when succeeding 
dilutions for preparation of calibration standards cannot be 
verified.
    CAUTION: Many of these chemicals are extremely toxic if inhaled 
or swallowed (Section 5.1). Wash hands thoroughly after handling.
    Typical stock solution preparation procedures follow for 1 L 
quantities, but for the purpose of pollution prevention, the analyst 
is encouraged to prepare smaller quantities when possible. 
Concentrations are calculated based upon the weight of the pure 
element or upon the weight of the compound multiplied by the 
fraction of the analyte in the compound
    From pure element,

[[Page 29817]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.001

where: gravimetric factor = the weight fraction of the analyte in 
the compound

    7.8.1 Aluminum solution, stock, 1 mL = 1000 [mu]g Al: Dissolve 
1.000 g of aluminum metal, weighed accurately to at least four 
significant figures, in an acid mixture of 4.0 mL of (1+1) HCl and 1 
mL of concentrated HNO3 in a beaker. Warm beaker slowly 
to effect solution. When dissolution is complete, transfer solution 
quantitatively to a 1 L flask, add an additional 10.0 mL of (1+1) 
HCl and dilute to volume with reagent water.
    7.8.2 Antimony solution, stock, 1 mL = 1000 [mu]g Sb: Dissolve 
1.000 g of antimony powder, weighed accurately to at least four 
significant figures, in 20.0 mL (1+1) HNO3 and 10.0 mL 
concentrated HCl. Add 100 mL reagent water and 1.50 g tartaric acid. 
Warm solution slightly to effect complete dissolution. Cool solution 
and add reagent water to volume in a 1 L volumetric flask.
    7.8.3 Arsenic solution, stock, 1 mL = 1000 [mu]g As: Dissolve 
1.320 g of As2O3 (As fraction = 0.7574), 
weighed accurately to at least four significant figures, in 100 mL 
of reagent water containing 10.0 mL concentrated NH4OH. 
Warm the solution gently to effect dissolution. Acidify the solution 
with 20.0 mL concentrated HNO3 and dilute to volume in a 
1 L volumetric flask with reagent water.
    7.8.4 Barium solution, stock, 1 mL = 1000 [mu]g Ba: Dissolve 
1.437 g BaCO3 (Ba fraction = 0.6960), weighed accurately 
to at least four significant figures, in 150 mL (1+2) 
HNO3 with heating and stirring to degas and dissolve 
compound. Let solution cool and dilute with reagent water in 1 L 
volumetric flask.
    7.8.5 Beryllium solution, stock, 1 mL = 1000 [mu]g Be: DO NOT 
DRY. Dissolve 19.66 g BeSO44H2O (Be 
fraction = 0.0509), weighed accurately to at least four significant 
figures, in reagent water, add 10.0 mL concentrated HNO3, 
and dilute to volume in a 1 L volumetric flask with reagent water.
    7.8.6 Boron solution, stock, 1 mL = 1000 [mu]g B: DO NOT DRY. 
Dissolve 5.716 g anhydrous H3BO3 (B fraction = 
0.1749), weighed accurately to at least four significant figures, in 
reagent water and dilute in a 1 L volumetric flask with reagent 
water. Transfer immediately after mixing to a clean FEP bottle to 
minimize any leaching of boron from the glass volumetric container. 
Use of a nonglass volumetric flask is recommended to avoid boron 
contamination from glassware.
    7.8.7 Cadmium solution, stock, 1 mL = 1000 [mu]g Cd: Dissolve 
1.000 g Cd metal, acid cleaned with (1+9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1+1) 
HNO3 with heating to effect dissolution. Let solution 
cool and dilute with reagent water in a 1 L volumetric flask.
    7.8.8 Calcium solution, stock, 1 mL = 1000 [mu]g Ca: Suspend 
2.498 g CaCO3 (Ca fraction = 0.4005), dried at 180 [deg]C 
for one hour before weighing, weighed accurately to at least four 
significant figures, in reagent water and dissolve cautiously with a 
minimum amount of (1+1) HNO3. Add 10.0 mL concentrated 
HNO3 and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.9 Cerium solution, stock, 1 mL = 1000 [mu]g Ce: Slurry 1.228 
g CeO2 (Ce fraction = 0.8141), weighed accurately to at 
least four significant figures, in 100 mL concentrated 
HNO3 and evaporate to dryness. Slurry the residue in 20 
mL H2O, add 50 mL concentrated HNO3, with heat 
and stirring add 60 mL 50% H2O2 dropwise in 1 
mL increments allowing periods of stirring between the 1 mL 
additions. Boil off excess H2O2 before 
diluting to volume in a 1 L volumetric flask with reagent water.
    7.8.10 Chromium solution, stock, 1 mL = 1000 [mu]g Cr: Dissolve 
1.923 g CrO3 (Cr fraction = 0.5200), weighed accurately 
to at least four significant figures, in 120 mL (1+5) 
HNO3. When solution is complete, dilute to volume in a 1 
L volumetric flask with reagent water.
    7.8.11 Cobalt solution, stock, 1 mL = 1000 [mu]g Co: Dissolve 
1.000 g Co metal, acid cleaned with (1+9) HNO3, weighed 
accurately to at least four significant figures, in 50.0 mL (1+1) 
HNO3. Let solution cool and dilute to volume in a 1 L 
volumetric flask with reagent water.
    7.8.12 Copper solution, stock, 1 mL = 1000 [mu]g Cu: Dissolve 
1.000 g Cu metal, acid cleaned with (1+9) HNO3, weighed 
accurately to at least four significant figures, in 50.0 mL (1+1) 
HNO3 with heating to effect dissolution. Let solution 
cool and dilute in a 1 L volumetric flask with reagent water.
    7.8.13 Iron solution, stock, 1 mL = 1000 [mu]g Fe: Dissolve 
1.000 g Fe metal, acid cleaned with (1+1) HCl, weighed accurately to 
four significant figures, in 100 mL (1+1) HCl with heating to effect 
dissolution. Let solution cool and dilute with reagent water in a 1 
L volumetric flask.
    7.8.14 Lead solution, stock, 1 mL = 1000 [mu]g Pb: Dissolve 
1.599 g Pb(NO3)2 (Pb fraction = 0.6256), 
weighed accurately to at least four significant figures, in a 
minimum amount of (1+1) HNO3. Add 20.0 mL (1+1) 
HNO3 and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.15 Lithium solution, stock, 1 mL = 1000 [mu]g Li: Dissolve 
5.324 g Li2CO3 (Li fraction = 0.1878), weighed 
accurately to at least four significant figures, in a minimum amount 
of (1+1) HCl and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.16 Magnesium solution, stock, 1 mL = 1000 [mu]g Mg: Dissolve 
1.000 g cleanly polished Mg ribbon, accurately weighed to at least 
four significant figures, in slowly added 5.0 mL (1+1) HCl (CAUTION: 
reaction is vigorous). Add 20.0 mL (1+1) HNO3 and dilute 
to volume in a 1 L volumetric flask with reagent water.
    7.8.17 Manganese solution, stock, 1 mL = 1000 [mu]g Mn: Dissolve 
1.000 g of manganese metal, weighed accurately to at least four 
significant figures, in 50 mL (1+1) HNO3 and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.18 Mercury solution, stock, 1 mL = 1000 [mu]g Hg: DO NOT 
DRY. CAUTION: highly toxic element. Dissolve 1.354 g 
HgCl2 (Hg fraction = 0.7388) in reagent water. Add 50.0 
mL concentrated HNO3 and dilute to volume in 1 L 
volumetric flask with reagent water.
    7.8.19 Molybdenum solution, stock, 1 mL = 1000 [mu]g Mo: 
Dissolve 1.500 g MoO3 (Mo fraction = 0.6666), weighed 
accurately to at least four significant figures, in a mixture of 100 
mL reagent water and 10.0 mL concentrated NH4OH, heating 
to effect dissolution. Let solution cool and dilute with reagent 
water in a 1 L volumetric flask.
    7.8.20 Nickel solution, stock, 1 mL = 1000 [mu]g Ni: Dissolve 
1.000 g of nickel metal, weighed accurately to at least four 
significant figures, in 20.0 mL hot concentrated HNO3, 
cool, and dilute to volume in a 1 L volumetric flask with reagent 
water.
    7.8.21 Phosphorus solution, stock, 1 mL = 1000 [mu]g P: Dissolve 
3.745 g NH4H2PO4 (P fraction = 
0.2696), weighed accurately to at least four significant figures, in 
200 mL reagent water and dilute to volume in a 1 L volumetric flask 
with reagent water.
    7.8.22 Potassium solution, stock, 1 mL = 1000 [mu]g K: Dissolve 
1.907 g KCl (K fraction = 0.5244) dried at 110 [deg]C, weighed 
accurately to at least four significant figures, in reagent water, 
add 20 mL (1+1) HCl and dilute to volume in a 1 L volumetric flask 
with reagent water.
    7.8.23 Selenium solution, stock, 1 mL = 1000 [mu]g Se: Dissolve 
1.405 g SeO2 (Se fraction = 0.7116), weighed accurately 
to at least four significant figures, in 200 mL reagent water and 
dilute to volume in a 1 L volumetric flask with reagent water.
    7.8.24 Silica solution, stock, 1 mL = 1000 [mu]g 
SiO2: DO NOT DRY. Dissolve 2.964 g 
(NH4)2SiF6, weighed accurately to 
at least four significant figures, in 200 mL (1+20) HCl with heating 
at 85 [deg]C to effect dissolution. Let solution cool and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.25 Silver solution, stock, 1 mL = 1000 [mu]g Ag: Dissolve 
1.000 g Ag metal, weighed accurately to at least four significant 
figures, in 80 mL (1+1) HNO3 with heating to effect 
dissolution. Let solution cool and dilute with reagent water in a 1 
L volumetric flask. Store

[[Page 29818]]

solution in amber bottle or wrap bottle completely with aluminum 
foil to protect solution from light.
    7.8.26 Sodium solution, stock, 1 mL = 1000 [mu]g Na: Dissolve 
2.542 g NaCl (Na fraction = 0.3934), weighed accurately to at least 
four significant figures, in reagent water. Add 10.0 mL concentrated 
HNO3 and dilute to volume in a 1 L volumetric flask with 
reagent water.
    7.8.27 Strontium solution, stock, 1 mL = 1000 [mu]g Sr: Dissolve 
1.685 g SrCO3 (Sr fraction = 0.5935), weighed accurately 
to at least four significant figures, in 200 mL reagent water with 
dropwise addition of 100 mL (1+1) HCl. Dilute to volume in a 1 L 
volumetric flask with reagent water.
    7.8.28 Thallium solution, stock, 1 mL = 1000 [mu]g Tl: Dissolve 
1.303 g TlNO3 (Tl fraction = 0.7672), weighed accurately 
to at least four significant figures, in reagent water. Add 10.0 mL 
concentrated HNO3 and dilute to volume in a 1 L 
volumetric flask with reagent water.
    7.8.29 Tin solution, stock, 1 mL = 1000 [mu]g Sn: Dissolve 1.000 
g Sn shot, weighed accurately to at least four significant figures, 
in an acid mixture of 10.0 mL concentrated HCl and 2.0 mL (1+1) 
HNO3 with heating to effect dissolution. Let solution 
cool, add 200 mL concentrated HCl, and dilute to volume in a 1 L 
volumetric flask with reagent water.
    7.8.30 Titanium solution, stock, 1 mL = 1000 [mu]g Ti: DO NOT 
DRY. Dissolve 6.138 g 
(NH4)2TiO(C2O4)2
H2O (Ti fraction = 0.1629), weighed accurately to 
at least four significant figures, in 100 mL reagent water. Dilute 
to volume in a 1 L volumetric flask with reagent water.
    7.8.31 Vanadium solution, stock, 1 mL = 1000 [mu]g V: Dissolve 
1.000 g V metal, acid cleaned with (1+9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1+1) 
HNO3 with heating to effect dissolution. Let solution 
cool and dilute with reagent water to volume in a 1 L volumetric 
flask.
    7.8.32 Yttrium solution, stock 1 mL = 1000 [mu]g Y: Dissolve 
1.270 g Y2O3 (Y fraction = 0.7875), weighed 
accurately to at least four significant figures, in 50 mL (1+1) 
HNO3, heating to effect dissolution. Cool and dilute to 
volume in a 1 L volumetric flask with reagent water.
    7.8.33 Zinc solution, stock, 1 mL = 1000 [mu]g Zn: Dissolve 
1.000 g Zn metal, acid cleaned with (1+9) HNO3, weighed 
accurately to at least four significant figures, in 50 mL (1+1) 
HNO3 with heating to effect dissolution. Let solution 
cool and dilute with reagent water to volume in a 1 L volumetric 
flask.
    7.9 Mixed Calibration Standard Solutions--For the analysis of 
total recoverable digested samples prepare mixed calibration 
standard solutions (see Table 3) by combining appropriate volumes of 
the stock solutions in 500 mL volumetric flasks containing 20 mL 
(1+1) HNO3 and 20 mL (1+1) HCl and dilute to volume with 
reagent water. Prior to preparing the mixed standards, each stock 
solution should be analyzed separately to determine possible 
spectral interferences or the presence of impurities. Care should be 
taken when preparing the mixed standards to ensure that the elements 
are compatible and stable together. To minimize the opportunity for 
contamination by the containers, it is recommended to transfer the 
mixed-standard solutions to acid-cleaned, never-used FEP 
fluorocarbon (FEP) bottles for storage. Fresh mixed standards should 
be prepared, as needed, with the realization that concentrations can 
change on aging. Calibration standards not prepared from primary 
standards must be initially verified using a certified reference 
solution. For the recommended wavelengths listed in Table 1 some 
typical calibration standard combinations are given in Table 3.
    Note: If the addition of silver to the recommended mixed-acid 
calibration standard results in an initial precipitation, add 15 mL 
of reagent water and warm the flask until the solution clears. For 
this acid combination, the silver concentration should be limited to 
0.5 mg/L.
    7.10 Blanks--Four types of blanks are required for the analysis. 
The calibration blank is used in establishing the analytical curve, 
the laboratory reagent blank is used to assess possible 
contamination from the sample preparation procedure, the laboratory 
fortified blank is used to assess routine laboratory performance and 
a rinse blank is used to flush the instrument uptake system and 
nebulizer between standards, check solutions, and samples to reduce 
memory interferences.
    7.10.1 The calibration blank for aqueous samples and extracts is 
prepared by acidifying reagent water to the same concentrations of 
the acids as used for the standards. The calibration blank should be 
stored in a FEP bottle.
    7.10.2 The laboratory reagent blank (LRB) must contain all the 
reagents in the same volumes as used in the processing of the 
samples. The LRB must be carried through the same entire preparation 
scheme as the samples including sample digestion, when applicable.
    7.10.3 The laboratory fortified blank (LFB) is prepared by 
fortifying an aliquot of the laboratory reagent blank with all 
analytes to a suitable concentration using the following recommended 
criteria: Ag 0.1 mg/L, K 5.0 mg/L and all other analytes 0.2 mg/L or 
a concentration approximately 100 times their respective MDL, 
whichever is greater. The LFB must be carried through the same 
entire preparation scheme as the samples including sample digestion, 
when applicable.
    7.10.4 The rinse blank is prepared by acidifying reagent water 
to the same concentrations of acids as used in the calibration blank 
and stored in a convenient manner.
    7.11 Instrument Performance Check (IPC) Solution--The IPC 
solution is used to periodically verify instrument performance 
during analysis. It should be prepared in the same acid mixture as 
the calibration standards by combining method analytes at 
appropriate concentrations. Silver must be limited to <0.5 mg/L; 
while potassium and phosphorus because of higher MDLs and silica 
because of potential contamination should be at concentrations of 10 
mg/L. For other analytes a concentration of 2 mg/L is recommended. 
The IPC solution should be prepared from the same standard stock 
solutions used to prepare the calibration standards and stored in an 
FEP bottle. Agency programs may specify or request that additional 
instrument performance check solutions be prepared at specified 
concentrations in order to meet particular program needs.
    7.12 Quality Control Sample (QCS)--Analysis of a QCS is required 
for initial and periodic verification of calibration standards or 
stock standard solutions in order to verify instrument performance. 
The QCS must be obtained from an outside source different from the 
standard stock solutions and prepared in the same acid mixture as 
the calibration standards. The concentration of the analytes in the 
QCS solution should be 1 mg/L, except silver, which must be limited 
to a concentration of 0.5 mg/L for solution stability. The QCS 
solution should be stored in a FEP bottle and analyzed as needed to 
meet data-quality needs. A fresh solution should be prepared 
quarterly or more frequently as needed.
    7.13 Spectral Interference Check (SIC) Solutions--When 
interelement corrections are applied, SIC solutions are needed 
containing concentrations of the interfering elements at levels that 
will provide an adequate test of the correction factors.
    7.13.1 SIC solutions containing (a) 300 mg/L Fe; (b) 200 mg/L 
AL; (c) 50 mg/L Ba; (d) 50 mg/L Be; (e) 50 mg/L Cd; (f) 50 mg/L Ce; 
(g) 50 mg/L Co; (h) 50 mg/L Cr; (i) 50 mg/L Cu; (j) 50 mg/L Mn; (k) 
50 mg/L Mo; (l) 50 mg/L Ni; (m) 50 mg/L Sn; (n) 50 mg/L 
SiO2; (o) 50 mg/L Ti; (p) 50 mg/L Tl and (q) 50 mg/L V 
should be prepared in the same acid mixture as the calibration 
standards and stored in FEP bottles. These solutions can be used to 
periodically verify a partial list of the on-line (and possible off-
line) interelement spectral correction factors for the recommended 
wavelengths given in Table 1. Other solutions could achieve the same 
objective as well. (Multielement SIC solutions\3\ may be prepared 
and substituted for the single element solutions provided an analyte 
is not subject to interference from more than one interferant in the 
solution.)
    Note: If wavelengths other than those recommended in Table 1 are 
used, other solutions different from those above (a through q) may 
be required.
    7.13.2 For interferences from iron and aluminum, only those 
correction factors (positive or negative) when multiplied by 100 to 
calculate apparent analyte concentrations that exceed the determined 
analyte IDL or fall below the lower 3-sigma control limit of the 
calibration blank need be tested on a daily basis.
    7.13.3 For the other interfering elements, only those correction 
factors (positive or negative) when multiplied by 10 to calculate 
apparent analyte concentrations that exceed the determined analyte 
IDL or fall below the lower 3-sigma control limit of the calibration 
blank need be tested on a daily basis.
    7.13.4 If the correction routine is operating properly, the 
determined apparent analyte(s) concentration from analysis of each 
interference solution (a through q) should fall within a specific 
concentration range bracketing the calibration blank. This

[[Page 29819]]

concentration range is calculated by multiplying the concentration 
of the interfering element by the value of the correction factor 
being tested and dividing by 10. If after subtraction of the 
calibration blank the apparent analyte concentration is outside 
(above or below) this range, a change in the correction factor of 
more than 10% should be suspected. The cause of the change should be 
determined and corrected and the correction factor should be 
updated.
    Note: The SIC solution should be analyzed more than once to 
confirm a change has occurred with adequate rinse time between 
solutions and before subsequent analysis of the calibration blank.
    7.13.5 If the correction factors tested on a daily basis are 
found to be within the 10% criteria for five consecutive days, the 
required verification frequency of those factors in compliance may 
be extended to a weekly basis. Also, if the nature of the samples 
analyzed is such (e.g., finished drinking water) that they do not 
contain concentrations of the interfering elements at the 10 mg/L 
level, daily verification is not required; however, all interelement 
spectral correction factors must be verified annually and updated, 
if necessary.
    7.13.6 If the instrument does not display negative concentration 
values, fortify the SIC solutions with the elements of interest at 1 
mg/L and test for analyte recoveries that are below 95%. In the 
absence of measurable analyte, over-correction could go undetected 
because a negative value could be reported as zero.
    7.14 For instruments without interelement correction capability 
or when interelement corrections are not used, SIC solutions 
(containing similar concentrations of the major components in the 
samples, e.g., 10 mg/L) can serve to verify the absence of effects 
at the wavelengths selected. These data must be kept on file with 
the sample analysis data. If the SIC solution confirms an operative 
interference that is 10% of the analyte concentration, the analyte 
must be determined using a wavelength and background correction 
location free of the interference or by another approved test 
procedure. Users are advised that high salt concentrations can cause 
analyte signal suppressions and confuse interference tests.
    7.15 Plasma Solution--The plasma solution is used for 
determining the optimum viewing height of the plasma above the work 
coil prior to using the method (Section 10.2). The solution is 
prepared by adding a 5 mL aliquot from each of the stock standard 
solutions of arsenic, lead, selenium, and thallium to a mixture of 
20 mL (1+1) nitric acid and 20 mL (1+1) hydrochloric acid and 
diluting to 500 mL with reagent water. Store in a FEP bottle.

8.0 Sample Collection, Preservation, and Storage

    8.1 Prior to the collection of an aqueous sample, consideration 
should be given to the type of data required, (i.e., dissolved or 
total recoverable), so that appropriate preservation and 
pretreatment steps can be taken. The pH of all aqueous samples must 
be tested immediately prior to aliquoting for processing or ``direct 
analysis'' to ensure the sample has been properly preserved. If 
properly acid preserved, the sample can be held up to six months 
before analysis.
    8.2 For the determination of the dissolved elements, the sample 
must be filtered through a 0.45 [mu]m pore diameter membrane filter 
at the time of collection or as soon thereafter as practically 
possible. (Glass or plastic filtering apparatus are recommended to 
avoid possible contamination. Only plastic apparatus should be used 
when the determinations of boron and silica are critical.) Use a 
portion of the filtered sample to rinse the filter flask, discard 
this portion and collect the required volume of filtrate. Acidify 
the filtrate with (1+1) nitric acid immediately following filtration 
to pH <2.
    8.3 For the determination of total recoverable elements in 
aqueous samples, samples are not filtered, but acidified with (1+1) 
nitric acid to pH <2 (normally, 3 mL of (1+1) acid per liter of 
sample is sufficient for most ambient and drinking water samples). 
Preservation may be done at the time of collection, however, to 
avoid the hazards of strong acids in the field, transport 
restrictions, and possible contamination it is recommended that the 
samples be returned to the laboratory within two weeks of collection 
and acid preserved upon receipt in the laboratory. Following 
acidification, the sample should be mixed, held for 16 hours, and 
then verified to be pH <2 just prior withdrawing an aliquot for 
processing or ``direct analysis''. If for some reason such as high 
alkalinity the sample pH is verified to be >2, more acid must be 
added and the sample held for 16 hours until verified to be pH <2. 
See Section 8.1.
    Note: When the nature of the sample is either unknown or is 
known to be hazardous, acidification should be done in a fume hood. 
See Section 5.2.
    8.4 Solid samples require no preservation prior to analysis 
other than storage at 4 [deg]C. There is no established holding time 
limitation for solid samples.
    8.5 For aqueous samples, a field blank should be prepared and 
analyzed as required by the data user. Use the same container and 
acid as used in sample collection.

9.0 Quality Control

    9.1 Each laboratory using this method is required to operate a 
formal quality control (QC) program. The minimum requirements of 
this program consist of an initial demonstration of laboratory 
capability, and the periodic analysis of laboratory reagent blanks, 
fortified blanks and other laboratory solutions as a continuing 
check on performance. The laboratory is required to maintain 
performance records that define the quality of the data thus 
generated.
    9.2 Initial Demonstration of Performance (mandatory).
    9.2.1 The initial demonstration of performance is used to 
characterize instrument performance (determination of linear dynamic 
ranges and analysis of quality control samples) and laboratory 
performance (determination of method detection limits) prior to 
analyses conducted by this method.
    9.2.2 Linear dynamic range (LDR)--The upper limit of the LDR 
must be established for each wavelength utilized. It must be 
determined from a linear calibration prepared in the normal manner 
using the established analytical operating procedure for the 
instrument. The LDR should be determined by analyzing succeedingly 
higher standard concentrations of the analyte until the observed 
analyte concentration is no more than 10% below the stated 
concentration of the standard. Determined LDRs must be documented 
and kept on file. The LDR which may be used for the analysis of 
samples should be judged by the analyst from the resulting data. 
Determined sample analyte concentrations that are greater than 90% 
of the determined upper LDR limit must be diluted and reanalyzed. 
The LDRs should be verified annually or whenever, in the judgment of 
the analyst, a change in analytical performance caused by either a 
change in instrument hardware or operating conditions would dictate 
they be redetermined.
    9.2.3 Quality control sample (QCS)--When beginning the use of 
this method, on a quarterly basis, after the preparation of stock or 
calibration standard solutions or as required to meet data-quality 
needs, verify the calibration standards and acceptable instrument 
performance with the preparation and analyses of a QCS (Section 
7.12). To verify the calibration standards the determined mean 
concentrations from three analyses of the QCS must be within 5% of 
the stated values. If the calibration standard cannot be verified, 
performance of the determinative step of the method is unacceptable. 
The source of the problem must be identified and corrected before 
either proceeding on with the initial determination of method 
detection limits or continuing with on-going analyses.
    9.2.4 Method detection limit (MDL)--MDLs must be established for 
all wavelengths utilized, using reagent water (blank) fortified at a 
concentration of two to three times the estimated instrument 
detection limit.\15\ To determine MDL values, take seven replicate 
aliquots of the fortified reagent water and process through the 
entire analytical method. Perform all calculations defined in the 
method and report the concentration values in the appropriate units. 
Calculate the MDL as follows:

MDL = (t) x (S)

Where:

t = students' t value for a 99% confidence level and a standard 
deviation estimate with n-1 degrees of freedom [t = 3.14 for seven 
replicates]
S = standard deviation of the replicate analyses

    Note: If additional confirmation is desired, reanalyze the seven 
replicate aliquots on two more nonconsecutive days and again 
calculate the MDL values for each day. An average of the three MDL 
values for each analyte may provide for a more appropriate MDL 
estimate. If the relative standard deviation (RSD) from the analyses 
of the seven aliquots is <10%, the concentration used to determine 
the analyte MDL may have been inappropriately high for the 
determination. If so, this could result in the calculation of an 
unrealistically low MDL. Concurrently, determination of MDL in

[[Page 29820]]

reagent water represents a best case situation and does not reflect 
possible matrix effects of real world samples. However, successful 
analyses of LFMs (Section 9.4) and the analyte addition test 
described in Section 9.5.1 can give confidence to the MDL value 
determined in reagent water. Typical single laboratory MDL values 
using this method are given in Table 4.
    The MDLs must be sufficient to detect analytes at the required 
levels according to compliance monitoring regulation (Section 1.2). 
MDLs should be determined annually, when a new operator begins work 
or whenever, in the judgment of the analyst, a change in analytical 
performance caused by either a change in instrument hardware or 
operating conditions would dictate they be redetermined.
    9.3 Assessing Laboratory Performance (mandatory)
    9.3.1 Laboratory reagent blank (LRB)--The laboratory must 
analyze at least one LRB (Section 7.10.2) with each batch of 20 or 
fewer samples of the same matrix. LRB data are used to assess 
contamination from the laboratory environment. LRB values that 
exceed the MDL indicate laboratory or reagent contamination should 
be suspected. When LRB values constitute 10% or more of the analyte 
level determined for a sample or is 2.2 times the analyte MDL 
whichever is greater, fresh aliquots of the samples must be prepared 
and analyzed again for the affected analytes after the source of 
contamination has been corrected and acceptable LRB values have been 
obtained.
    9.3.2 Laboratory fortified blank (LFB)--The laboratory must 
analyze at least one LFB (Section 7.10.3) with each batch of 
samples. Calculate accuracy as percent recovery using the following 
equation:
[GRAPHIC] [TIFF OMITTED] TR18MY12.002

Where:

R = percent recovery
LFB = laboratory fortified blank
LRB = laboratory reagent blank
s = concentration equivalent of analyte added to fortify the LBR 
solution

    If the recovery of any analyte falls outside the required 
control limits of 85-115%, that analyte is judged out of control, 
and the source of the problem should be identified and resolved 
before continuing analyses.
    9.3.3 The laboratory must use LFB analyses data to assess 
laboratory performance against the required control limits of 85-
115% (Section 9.3.2). When sufficient internal performance data 
become available (usually a minimum of 20-30 analyses), optional 
control limits can be developed from the mean percent recovery (x) 
and the standard deviation (S) of the mean percent recovery. These 
data can be used to establish the upper and lower control limits as 
follows:

UPPER CONTROL LIMIT = x + 3S
LOWER CONTROL LIMIT = x - 3S

    The optional control limits must be equal to or better than the 
required control limits of 85-115%. After each five to 10 new 
recovery measurements, new control limits can be calculated using 
only the most recent 20-30 data points. Also, the standard deviation 
(S) data should be used to establish an on-going precision statement 
for the level of concentrations included in the LFB. These data must 
be kept on file and be available for review.
    9.3.4 Instrument performance check (IPC) solution--For all 
determinations the laboratory must analyze the IPC solution (Section 
7.11) and a calibration blank immediately following daily 
calibration, after every 10th sample (or more frequently, if 
required) and at the end of the sample run. Analysis of the 
calibration blank should always be < the analyte IDL, but greater 
than the lower 3-sigma control limit of the calibration blank. 
Analysis of the IPC solution immediately following calibration must 
verify that the instrument is within 5% of calibration with a 
relative standard deviation <3% from replicate integrations 4. 
Subsequent analyses of the IPC solution must be within 10% of 
calibration. If the calibration cannot be verified within the 
specified limits, reanalyze either or both the IPC solution and the 
calibration blank. If the second analysis of the IPC solution or the 
calibration blank confirm calibration to be outside the limits, 
sample analysis must be discontinued, the cause determined, 
corrected and/or the instrument recalibrated. All samples following 
the last acceptable IPC solution must be reanalyzed. The analysis 
data of the calibration blank and IPC solution must be kept on file 
with the sample analyses data.
    9.3.5 Spectral interference check (SIC) solution--For all 
determinations the laboratory must periodically verify the 
interelement spectral interference correction routine by analyzing 
SIC solutions. The preparation and required periodic analysis of SIC 
solutions and test criteria for verifying the interelement 
interference correction routine are given in Section 7.13. Special 
cases where on-going verification is required are described in 
Section 7.14.
    9.4 Assessing Analyte Recovery and Data Quality.
    9.4.1 Sample homogeneity and the chemical nature of the sample 
matrix can affect analyte recovery and the quality of the data. 
Taking separate aliquots from the sample for replicate and fortified 
analyses can in some cases assess the effect. Unless otherwise 
specified by the data user, laboratory or program, the following 
laboratory fortified matrix (LFM) procedure (Section 9.4.2) is 
required. Also, other tests such as the analyte addition test 
(Section 9.5.1) and sample dilution test (Section 9.5.2) can 
indicate if matrix effects are operative.
    9.4.2 The laboratory must add a known amount of each analyte to 
a minimum of 10% of the routine samples. In each case the LFM 
aliquot must be a duplicate of the aliquot used for sample analysis 
and for total recoverable determinations added prior to sample 
preparation. For water samples, the added analyte concentration must 
be the same as that used in the laboratory fortified blank (Section 
7.10.3). For solid samples, however, the concentration added should 
be expressed as mg/kg and is calculated for a one gram aliquot by 
multiplying the added analyte concentration (mg/L) in solution by 
the conversion factor 100 (mg/L x 0.1L/0.001kg = 100, Section 12.5). 
(For notes on Ag, Ba, and Sn see Sections 1.7 and 1.8.) Over time, 
samples from all routine sample sources should be fortified.
    Note: The concentration of calcium, magnesium, sodium and 
strontium in environmental waters, along with iron and aluminum in 
solids can vary greatly and are not necessarily predictable. 
Fortifying these analytes in routine samples at the same 
concentration used for the LFB may prove to be of little use in 
assessing data quality for these analytes. For these analytes sample 
dilution and reanalysis using the criteria given in Section 9.5.2 is 
recommended. Also, if specified by the data user, laboratory or 
program, samples can be fortified at higher concentrations, but even 
major constituents should be limited to <25 mg/L so as not to alter 
the sample matrix and affect the analysis.
    9.4.3 Calculate the percent recovery for each analyte, corrected 
for background concentrations measured in the unfortified sample, 
and compare these values to the designated LFM recovery range of 70-
130% or a 3-sigma recovery range calculated from the regression 
equations given in Table 9.\16\ Recovery calculations are not 
required if the concentration added is less than 30% of the sample 
background concentration. Percent recovery may be calculated in 
units appropriate to the matrix, using the following equation:
[GRAPHIC] [TIFF OMITTED] TR18MY12.003

Where:

R = percent recovery
Cs = fortified sample concentration
C = sample background concentration
s = concentration equivalent of analyte added to fortify the sample

    9.4.4 If the recovery of any analyte falls outside the 
designated LFM recovery range, and the laboratory performance for 
that analyte is shown to be in control (Section 9.3), the recovery 
problem encountered with the fortified sample is judged to be matrix 
related, not system related. The data user should be informed that 
the result for that analyte in the unfortified sample is suspect due 
to either the heterogeneous nature of the sample or matrix effects 
and analysis by method of standard addition or the use of an 
internal standard(s) (Section 11.5) should be considered.
    9.4.5 Where reference materials are available, they should be 
analyzed to provide additional performance data. The analysis of 
reference samples is a valuable tool for demonstrating the ability 
to perform the method acceptably. Reference materials containing 
high concentrations of analytes can provide additional information 
on the performance of the spectral interference correction routine.
    9.5 Assess the possible need for the method of standard 
additions (MSA) or internal standard elements by the following 
tests. Directions for using MSA or internal standard(s) are given in 
Section 11.5.
    9.5.1 Analyte addition test: An analyte(s) standard added to a 
portion of a prepared

[[Page 29821]]

sample, or its dilution, should be recovered to within 85% to 115% 
of the known value. The analyte(s) addition should produce a minimum 
level of 20 times and a maximum of 100 times the method detection 
limit. If the analyte addition is <20% of the sample analyte 
concentration, the following dilution test should be used. If 
recovery of the analyte(s) is not within the specified limits, a 
matrix effect should be suspected, and the associated data flagged 
accordingly. The method of additions or the use of an appropriate 
internal standard element may provide more accurate data.
    9.5.2 Dilution test: If the analyte concentration is 
sufficiently high (minimally, a factor of 50 above the instrument 
detection limit in the original solution but <90% of the linear 
limit), an analysis of a 1 + 4 dilution should agree (after 
correction for the fivefold dilution) within 10% of the original 
determination. If not, a chemical or physical interference effect 
should be suspected and the associated data flagged accordingly. The 
method of standard additions or the use of an internal-standard 
element may provide more accurate data for samples failing this 
test.

10.0 Calibration and Standardization

    10.1 Specific wavelengths are listed in Table 1. Other 
wavelengths may be substituted if they can provide the needed 
sensitivity and are corrected for spectral interference. However, 
because of the difference among various makes and models of 
spectrometers, specific instrument operating conditions cannot be 
given. The instrument and operating conditions utilized for 
determination must be capable of providing data of acceptable 
quality to the program and data user. The analyst should follow the 
instructions provided by the instrument manufacturer unless other 
conditions provide similar or better performance for a task. 
Operating conditions for aqueous solutions usually vary from 1100-
1200 watts forward power, 15-16 mm viewing height, 15-19 L/min. 
argon coolant flow, 0.6-1 L/min. argon aerosol flow, 1-1.8 mL/min. 
sample pumping rate with a one minute preflush time and measurement 
time near 1 s per wavelength peak (for sequential instruments) and 
near 10 s per sample (for simultaneous instruments). Use of the Cu/
Mn intensity ratio at 324.754 nm and 257.610 nm (by adjusting the 
argon aerosol flow) has been recommended as a way to achieve 
repeatable interference correction factors.\17\
    10.2 Prior to using this method optimize the plasma operating 
conditions. The following procedure is recommended for vertically 
configured plasmas. The purpose of plasma optimization is to provide 
a maximum signal-to-background ratio for the least sensitive element 
in the analytical array. The use of a mass flow controller to 
regulate the nebulizer gas flow rate greatly facilitates the 
procedure.
    10.2.1 Ignite the plasma and select an appropriate incident rf 
power with minimum reflected power. Allow the instrument to become 
thermally stable before beginning. This usually requires at least 30 
to 60 minutes of operation. While aspirating the 1000 [mu]g/mL 
solution of yttrium (Section 7.8.32), follow the instrument 
manufacturer's instructions and adjust the aerosol carrier gas flow 
rate through the nebulizer so a definitive blue emission region of 
the plasma extends approximately from 5-20 mm above the top of the 
work coil.\18\ Record the nebulizer gas flow rate or pressure 
setting for future reference.
    10.2.2 After establishing the nebulizer gas flow rate, determine 
the solution uptake rate of the nebulizer in mL/min. by aspirating a 
known volume calibration blank for a period of at least three 
minutes. Divide the spent volume by the aspiration time (in minutes) 
and record the uptake rate. Set the peristaltic pump to deliver the 
uptake rate in a steady even flow.
    10.2.3 After horizontally aligning the plasma and/or optically 
profiling the spectrometer, use the selected instrument conditions 
from Sections 10.2.1 and 10.2.2, and aspirate the plasma solution 
(Section 7.15), containing 10 [mu]g/mL each of As, Pb, Se and Tl. 
Collect intensity data at the wavelength peak for each analyte at 1 
mm intervals from 14-18 mm above the top of the work coil. (This 
region of the plasma is commonly referred to as the analytical 
zone.)\19\ Repeat the process using the calibration blank. Determine 
the net signal to blank intensity ratio for each analyte for each 
viewing height setting. Choose the height for viewing the plasma 
that provides the largest intensity ratio for the least sensitive 
element of the four analytes. If more than one position provides the 
same ratio, select the position that provides the highest net 
intensity counts for the least sensitive element or accept a 
compromise position of the intensity ratios of all four analytes.
    10.2.4 The instrument operating condition finally selected as 
being optimum should provide the lowest reliable instrument 
detection limits and method detection limits. Refer to Tables 1 and 
4 for comparison of IDLs and MDLs, respectively.
    10.2.5 If either the instrument operating conditions, such as 
incident power and/or nebulizer gas flow rate are changed, or a new 
torch injector tube having a different orifice i.d. is installed, 
the plasma and plasma viewing height should be reoptimized.
    10.2.6 Before daily calibration and after the instrument warmup 
period, the nebulizer gas flow must be reset to the determined 
optimized flow. If a mass flow controller is being used, it should 
be reset to the recorded optimized flow rate. In order to maintain 
valid spectral interelement correction routines the nebulizer gas 
flow rate should be the same from day-to-day (<2% change). The 
change in signal intensity with a change in nebulizer gas flow rate 
for both ``hard'' (Pb 220.353 nm) and ``soft'' (Cu 324.754) lines is 
illustrated in Figure 1.
    10.3 Before using the procedure (Section 11.0) to analyze 
samples, there must be data available documenting initial 
demonstration of performance. The required data and procedure is 
described in Section 9.2. This data must be generated using the same 
instrument operating conditions and calibration routine (Section 
11.4) to be used for sample analysis. These documented data must be 
kept on file and be available for review by the data user.
    10.4 After completing the initial demonstration of performance, 
but before analyzing samples, the laboratory must establish and 
initially verify an interelement spectral interference correction 
routine to be used during sample analysis. A general description 
concerning spectral interference and the analytical requirements for 
background correction and for correction of interelement spectral 
interference in particular are given in Section 4.1. To determine 
the appropriate location for background correction and to establish 
the interelement interference correction routine, repeated spectral 
scan about the analyte wavelength and repeated analyses of the 
single element solutions may be required. Criteria for determining 
an interelement spectral interference is an apparent positive or 
negative concentration on the analyte that is outside the 3-sigma 
control limits of the calibration blank for the analyte. (The upper-
control limit is the analyte IDL.) Once established, the entire 
routine must be initially and periodically verified annually, or 
whenever there is a change in instrument operating conditions 
(Section 10.2.5). Only a portion of the correction routine must be 
verified more frequently or on a daily basis. Test criteria and 
required solutions are described in Section 7.13. Initial and 
periodic verification data of the routine should be kept on file. 
Special cases where on-going verification are required is described 
in Section 7.14.

11.0 Procedure

11.1 Aqueous Sample Preparation--Dissolved Analytes

    11.1.1 For the determination of dissolved analytes in ground and 
surface waters, pipet an aliquot (20 mL) of the filtered, acid 
preserved sample into a 50 mL polypropylene centrifuge tube. Add an 
appropriate volume of (1 + 1) nitric acid to adjust the acid 
concentration of the aliquot to approximate a 1% (v[sol]v) nitric 
acid solution (e.g., add 0.4 mL (1 + 1) HNO3 to a 20 mL 
aliquot of sample). Cap the tube and mix. The sample is now ready 
for analysis (Section 1.3). Allowance for sample dilution should be 
made in the calculations. (If mercury is to be determined, a 
separate aliquot must be additionally acidified to contain 1% 
(v[sol]v) HCl to match the signal response of mercury in the 
calibration standard and reduce memory interference effects. Section 
1.9).
    Note: If a precipitate is formed during acidification, 
transport, or storage, the sample aliquot must be treated using the 
procedure described in Sections 11.2.2 through 11.2.7 prior to 
analysis.

11.2 Aqueous Sample Preparation--Total Recoverable Analytes

    11.2.1 For the ``direct analysis'' of total recoverable analytes 
in drinking water samples containing turbidity <1 NTU, treat an 
unfiltered acid preserved sample aliquot using the sample 
preparation procedure described in Section 11.1.1 while making 
allowance for sample dilution in the data calculation (Section 1.2). 
For the determination of total recoverable analytes in all other 
aqueous samples or for

[[Page 29822]]

preconcentrating drinking water samples prior to analysis follow the 
procedure given in Sections 11.2.2 through 11.2.7.
    11.2.2 For the determination of total recoverable analytes in 
aqueous samples (other than drinking water with <1 NTU turbidity), 
transfer a 100 mL (1 mL) aliquot from a well mixed, acid preserved 
sample to a 250 mL Griffin beaker (Sections 1.2, 1.3, 1.6, 1.7, 1.8, 
and 1.9). (When necessary, smaller sample aliquot volumes may be 
used.)
    Note: If the sample contains undissolved solids >1%, a well 
mixed, acid preserved aliquot containing no more than 1 g 
particulate material should be cautiously evaporated to near 10 mL 
and extracted using the acid-mixture procedure described in Sections 
11.3.3 through 11.3.6.
    11.2.3 Add 2 mL (1+1) nitric acid and 1.0 mL of (1+1) 
hydrochloric acid to the beaker containing the measured volume of 
sample. Place the beaker on the hot plate for solution evaporation. 
The hot plate should be located in a fume hood and previously 
adjusted to provide evaporation at a temperature of approximately 
but no higher than 85 [deg]C. (See the following note.) The beaker 
should be covered with an elevated watch glass or other necessary 
steps should be taken to prevent sample contamination from the fume 
hood environment.
    Note: For proper heating adjust the temperature control of the 
hot plate such that an uncovered Griffin beaker containing 50 mL of 
water placed in the center of the hot plate can be maintained at a 
temperature approximately but no higher than 85 [deg]C. (Once the 
beaker is covered with a watch glass the temperature of the water 
will rise to approximately 95 [deg]C.)
    11.2.4 Reduce the volume of the sample aliquot to about 20 mL by 
gentle heating at 85 [deg]C. DO NOT BOIL. This step takes about two 
hours for a 100 mL aliquot with the rate of evaporation rapidly 
increasing as the sample volume approaches 20 mL. (A spare beaker 
containing 20 mL of water can be used as a gauge.)
    11.2.5 Cover the lip of the beaker with a watch glass to reduce 
additional evaporation and gently reflux the sample for 30 minutes. 
(Slight boiling may occur, but vigorous boiling must be avoided to 
prevent loss of the HCl-H2O azeotrope.)
    11.2.6 Allow the beaker to cool. Quantitatively transfer the 
sample solution to a 50 mL volumetric flask, make to volume with 
reagent water, stopper and mix.
    11.2.7 Allow any undissolved material to settle overnight, or 
centrifuge a portion of the prepared sample until clear. (If after 
centrifuging or standing overnight the sample contains suspended 
solids that would clog the nebulizer, a portion of the sample may be 
filtered for their removal prior to analysis. However, care should 
be exercised to avoid potential contamination from filtration.) The 
sample is now ready for analysis. Because the effects of various 
matrices on the stability of diluted samples cannot be 
characterized, all analyses should be performed as soon as possible 
after the completed preparation.

11.3 Solid Sample Preparation--Total Recoverable Analytes

    11.3.1 For the determination of total recoverable analytes in 
solid samples, mix the sample thoroughly and transfer a portion (>20 
g) to tared weighing dish, weigh the sample and record the wet 
weight (WW). (For samples with <35% moisture a 20 g portion is 
sufficient. For samples with moisture >35% a larger aliquot 50-100 g 
is required.) Dry the sample to a constant weight at 60 [deg]C and 
record the dry weight (DW) for calculation of percent solids 
(Section 12.6). (The sample is dried at 60 [deg]C to prevent the 
loss of mercury and other possible volatile metallic compounds, to 
facilitate sieving, and to ready the sample for grinding.)
    11.3.2 To achieve homogeneity, sieve the dried sample using a 5-
mesh polypropylene sieve and grind in a mortar and pestle. (The 
sieve, mortar and pestle should be cleaned between samples.) From 
the dried, ground material weigh accurately a representative 1.0 
 0.01 g aliquot (W) of the sample and transfer to a 250 
mL Phillips beaker for acid extraction (Sections 1.6, 1.7, 1.8, and 
1.9).
    11.3.3 To the beaker add 4 mL of (1+1) HNO3 and 10 mL 
of (1+4) HCl. Cover the lip of the beaker with a watch glass. Place 
the beaker on a hot plate for reflux extraction of the analytes. The 
hot plate should be located in a fume hood and previously adjusted 
to provide a reflux temperature of approximately 95 [deg]C. (See the 
following note.)
    Note: For proper heating adjust the temperature control of the 
hot plate such that an uncovered Griffin beaker containing 50 mL of 
water placed in the center of the hot plate can be maintained at a 
temperature approximately but no higher than 85 [deg]C. (Once the 
beaker is covered with a watch glass the temperature of the water 
will rise to approximately 95 [deg]C.) Also, a block digester 
capable of maintaining a temperature of 95 [deg]C and equipped with 
250 mL constricted volumetric digestion tubes may be substituted for 
the hot plate and conical beakers in the extraction step.
    11.3.4 Heat the sample and gently reflux for 30 minutes. Very 
slight boiling may occur, however vigorous boiling must be avoided 
to prevent loss of the HCl-H2O azeotrope. Some solution 
evaporation will occur (3-4 mL).
    11.3.5 Allow the sample to cool and quantitatively transfer the 
extract to a 100 mL volumetric flask. Dilute to volume with reagent 
water, stopper and mix.
    11.3.6 Allow the sample extract solution to stand overnight to 
separate insoluble material or centrifuge a portion of the sample 
solution until clear. (If after centrifuging or standing overnight 
the extract solution contains suspended solids that would clog the 
nebulizer, a portion of the extract solution may be filtered for 
their removal prior to analysis. However, care should be exercised 
to avoid potential contamination from filtration.) The sample 
extract is now ready for analysis. Because the effects of various 
matrices on the stability of diluted samples cannot be 
characterized, all analyses should be performed as soon as possible 
after the completed preparation.

11.4 Sample Analysis

    11.4.1 Prior to daily calibration of the instrument inspect the 
sample introduction system including the nebulizer, torch, injector 
tube and uptake tubing for salt deposits, dirt and debris that would 
restrict solution flow and affect instrument performance. Clean the 
system when needed or on a daily basis.
    11.4.2 Configure the instrument system to the selected power and 
operating conditions as determined in Sections 10.1 and 10.2.
    11.4.3 The instrument must be allowed to become thermally stable 
before calibration and analyses. This usually requires at least 30 
to 60 minutes of operation. After instrument warmup, complete any 
required optical profiling or alignment particular to the 
instrument.
    11.4.4 For initial and daily operation calibrate the instrument 
according to the instrument manufacturer's recommended procedures, 
using mixed calibration standard solutions (Section 7.9) and the 
calibration blank (Section 7.10.1). A peristaltic pump must be used 
to introduce all solutions to the nebulizer. To allow equilibrium to 
be reached in the plasma, aspirate all solutions for 30 seconds 
after reaching the plasma before beginning integration of the 
background corrected signal to accumulate data. When possible, use 
the average value of replicate integration periods of the signal to 
be correlated to the analyte concentration. Flush the system with 
the rinse blank (Section 7.10.4) for a minimum of 60 seconds 
(Section 4.4) between each standard. The calibration line should 
consist of a minimum of a calibration blank and a high standard. 
Replicates of the blank and highest standard provide an optimal 
distribution of calibration standards to minimize the confidence 
band for a straight-line calibration in a response region with 
uniform variance.\20\
    11.4.5 After completion of the initial requirements of this 
method (Sections 10.3 and 10.4), samples should be analyzed in the 
same operational manner used in the calibration routine with the 
rinse blank also being used between all sample solutions, LFBs, 
LFMs, and check solutions (Section 7.10.4).
    11.4.6 During the analysis of samples, the laboratory must 
comply with the required quality control described in Sections 9.3 
and 9.4. Only for the determination of dissolved analytes or the 
``direct analysis'' of drinking water with turbidity of <1 NTU is 
the sample digestion step of the LRB, LFB, and LFM not required.
    11.4.7 Determined sample analyte concentrations that are 90% or 
more of the upper limit of the analyte LDR must be diluted with 
reagent water that has been acidified in the same manner as 
calibration blank and reanalyzed (see Section 11.4.8). Also, for the 
interelement spectral interference correction routines to remain 
valid during sample analysis, the interferant concentration must not 
exceed its LDR. If the interferant LDR is exceeded, sample dilution 
with acidified reagent water and reanalysis is required. In these 
circumstances analyte detection limits are raised and determination 
by another approved test procedure that is either more sensitive 
and/or interference free is recommended.

[[Page 29823]]

    11.4.8 When it is necessary to assess an operative matrix 
interference (e.g., signal reduction due to high dissolved solids), 
the tests described in Section 9.5 are recommended.
    11.4.9 Report data as directed in Section 12.0.
    11.5 If the method of standard additions (MSA) is used, 
standards are added at one or more levels to portions of a prepared 
sample. This technique \21\ compensates for enhancement or 
depression of an analyte signal by a matrix. It will not correct for 
additive interferences such as contamination, interelement 
interferences, or baseline shifts. This technique is valid in the 
linear range when the interference effect is constant over the 
range, the added analyte responds the same as the endogenous 
analyte, and the signal is corrected for additive interferences. The 
simplest version of this technique is the single-addition method. 
This procedure calls for two identical aliquots of the sample 
solution to be taken. To the first aliquot, a small volume of 
standard is added; while to the second aliquot, a volume of acid 
blank is added equal to the standard addition. The sample 
concentration is calculated by the following:
[GRAPHIC] [TIFF OMITTED] TR18MY12.004

Where:

C = Concentration of the standard solution (mg/L)
S1 = Signal for fortified aliquot
S2 = Signal for unfortified aliquot
V1 = Volume of the standard addition (L)
V2 = Volume of the sample aliquot (L) used for MSA

    For more than one fortified portion of the prepared sample, 
linear regression analysis can be applied using a computer or 
calculator program to obtain the concentration of the sample 
solution. An alternative to using the method of standard additions 
is use of the internal standard technique by adding one or more 
elements (not in the samples and verified not to cause an 
uncorrected interelement spectral interference) at the same 
concentration (which is sufficient for optimum precision) to the 
prepared samples (blanks and standards) that are affected the same 
as the analytes by the sample matrix. Use the ratio of analyte 
signal to the internal standard signal for calibration and 
quantitation.

12.0 Data Analysis and Calculations

    12.1 Sample data should be reported in units of mg/L for aqueous 
samples and mg/kg dry weight for solid samples.
    12.2 For dissolved aqueous analytes (Section 11.1) report the 
data generated directly from the instrument with allowance for 
sample dilution. Do not report analyte concentrations below the IDL.
    12.3 For total recoverable aqueous analytes (Section 11.2), 
multiply solution analyte concentrations by the dilution factor 0.5, 
when 100 mL aliquot is used to produce the 50 mL final solution, and 
report data as instructed in Section 12.4. If a different aliquot 
volume other than 100 mL is used for sample preparation, adjust the 
dilution factor accordingly. Also, account for any additional 
dilution of the prepared sample solution needed to complete the 
determination of analytes exceeding 90% or more of the LDR upper 
limit. Do not report data below the determined analyte MDL 
concentration or below an adjusted detection limit reflecting 
smaller sample aliquots used in processing or additional dilutions 
required to complete the analysis.
    12.4 For analytes with MDLs <0.01 mg/L, round the data values to 
the thousandth place and report analyte concentrations up to three 
significant figures. For analytes with MDLs <0.01 mg/L round the 
data values to the 100th place and report analyte concentrations up 
to three significant figures. Extract concentrations for solids data 
should be rounded in a similar manner before calculations in Section 
12.5 are performed.
    12.5 For total recoverable analytes in solid samples (Section 
11.3), round the solution analyte concentrations (mg/L) as 
instructed in Section 12.4. Report the data up to three significant 
figures as mg/kg dry-weight basis unless specified otherwise by the 
program or data user. Calculate the concentration using the equation 
below:
[GRAPHIC] [TIFF OMITTED] TR18MY12.005

Where:

C = Concentration in extract (mg/L)
V = Volume of extract (L, 100 mL = 0.1L)
D = Dilution factor (undiluted = 1)
W = Weight of sample aliquot extracted (g x 0.001 = kg)

    Do not report analyte data below the estimated solids MDL or an 
adjusted MDL because of additional dilutions required to complete 
the analysis.
    12.6 To report percent solids in solid samples (Section 11.3) 
calculate as follows:
[GRAPHIC] [TIFF OMITTED] TR18MY12.006

Where:

DW = Sample weight (g) dried at 60 [ordm]C
WW = Sample weight (g) before drying

    Note: If the data user, program or laboratory requires that the 
reported percent solids be determined by drying at 105 [deg]C, 
repeat the procedure given in Section 11.3 using a separate portion 
(>20 g) of the sample and dry to constant weight at 103-105 [deg]C.
    12.7 The QC data obtained during the analyses provide an 
indication of the quality of the sample data and should be provided 
with the sample results.

13.0 Method Performance

    13.1 Listed in Table 4 are typical single laboratory total 
recoverable MDLs determined for the recommended wavelengths using 
simultaneous ICP-AES and the operating conditions given in Table 5. 
The MDLs were determined in reagent blank matrix (best case 
situation). PTFE beakers were used to avoid boron and silica 
contamination from glassware with the final dilution to 50 mL 
completed in polypropylene centrifuged tubes. The listed MDLs for 
solids are estimates and were calculated from the aqueous MDL 
determinations.
    13.2 Data obtained from single laboratory method testing are 
summarized in Table 6 for five types of water samples consisting of 
drinking water, surface water, ground water, and two wastewater 
effluents. The data presented cover all analytes except cerium and 
titanium. Samples were prepared using the procedure described in 
Section 11.2. For each matrix, five replicate aliquots were 
prepared, analyzed and the average of the five determinations used 
to define the sample background concentration of each analyte. In 
addition, two pairs of duplicates were fortified at different 
concentration levels. For each method analyte, the sample background 
concentration, mean percent recovery, standard deviation of the 
percent recovery, and relative percent difference between the 
duplicate fortified samples are listed in Table 6. The variance of 
the five replicate sample background determinations is included in 
the calculated standard deviation of the percent recovery when the 
analyte concentration in the sample was greater than the MDL. The 
tap and well waters were processed in Teflon and quartz beakers and 
diluted in polypropylene centrifuged tubes. The nonuse of 
borosilicate glassware is reflected in the precision and recovery 
data for boron and silica in those two sample types.
    13.3 Data obtained from single laboratory method testing are 
summarized in Table 7 for three solid samples consisting of EPA 884 
Hazardous Soil, SRM 1645 River Sediment, and EPA 286 Electroplating 
Sludge. Samples were prepared using the procedure described in 
Section 11.3. For each method analyte, the sample background 
concentration, mean percent recovery of the fortified additions, the 
standard deviation of the percent

[[Page 29824]]

recovery, and relative percent difference between duplicate 
additions were determined as described in Section 13.2. Data 
presented are for all analytes except cerium, silica, and titanium. 
Limited comparative data to other methods and SRM materials are 
presented in Reference 23 of Section 16.0.
    13.4 Performance data for aqueous solutions independent of 
sample preparation from a multilaboratory study are provided in 
Table 8.\22\
    13.5 Listed in Table 9 are regression equations for precision 
and bias for 25 analytes abstracted from EPA Method Study 27, a 
multilaboratory validation study of Method 200.7.\1\ These equations 
were developed from data received from 12 laboratories using the 
total recoverable sample preparation procedure on reagent water, 
drinking water, surface water and three industrial effluents. For a 
complete review and description of the study, see Reference 16 of 
Section 16.0.

14.0 Pollution Prevention

    14.1 Pollution prevention encompasses any technique that reduces 
or eliminates the quantity or toxicity of waste at the point of 
generation. Numerous opportunities for pollution prevention exist in 
laboratory operation. The EPA has established a preferred hierarchy 
of environmental management techniques that places pollution 
prevention as the management option of first choice. Whenever 
feasible, laboratory personnel should use pollution prevention 
techniques to address their waste generation (e.g., Section 7.8). 
When wastes cannot be feasibly reduced at the source, the Agency 
recommends recycling as the next best option.
    14.2 For information about pollution prevention that may be 
applicable to laboratories and research institutions, consult ``Less 
is Better: Laboratory Chemical Management for Waste Reduction'', 
available from the American Chemical Society's Department of 
Government Relations and Science Policy, 1155 16th Street NW., 
Washington, DC 20036, (202) 872-4477.

15.0 Waste Management

    15.1 The Environmental Protection Agency requires that 
laboratory waste management practices be conducted consistent with 
all applicable rules and regulations. The Agency urges laboratories 
to protect the air, water, and land by minimizing and controlling 
all releases from hoods and bench operations, complying with the 
letter and spirit of any sewer discharge permits and regulations, 
and by complying with all solid and hazardous waste regulations, 
particularly the hazardous waste identification rules and land 
disposal restrictions. For further information on waste management 
consult ``The Waste Management Manual for Laboratory Personnel'', 
available from the American Chemical Society at the address listed 
in the Section 14.2.

16.0 References

1. U.S. Environmental Protection Agency. Inductively Coupled Plasma--
Atomic Emission Spectrometric Method for Trace Element Analysis of 
Water and Wastes--Method 200.7, Dec. 1982. EPA-600/4-79-020, revised 
March 1983.
2. U.S. Environmental Protection Agency. Inductively Coupled Plasma 
Atomic Emission Spectroscopy Method 6010, SW-846 Test Methods for 
Evaluating Solid Waste, 3rd Edition, 1986.
3. U.S. Environmental Protection Agency. Method 200.7: Determination of 
Metals and Trace Elements in Water and Wastes by Inductively Coupled 
Plasma--Atomic Emission Spectrometry, revision 3.3, EPA 600 4-91/010, 
June 1991.
4. U.S. Environmental Protection Agency. Inductively Coupled Plasma--
Atomic Emission Spectrometry Method for the Analysis of Waters and 
Solids, EMMC, July 1992.
5. Fassel, V.A. et al. Simultaneous Determination of Wear Metals in 
Lubricating Oils by Inductively-Coupled Plasma Atomic Emission 
Spectrometry. Anal. Chem. 48:516-519, 1976.
6. Merryfield, R.N. and R.C. Loyd. Simultaneous Determination of Metals 
in Oil by Inductively Coupled Plasma Emission Spectrometry. Anal. Chem. 
51:1965-1968, 1979.
7. Winge, R.K. et al. Inductively Coupled Plasma--Atomic Emission 
Spectroscopy: An Atlas of Spectral Information, Physical Science Data 
20. Elsevier Science Publishing, New York, New York, 1985.
8. Boumans, P.W.J.M. Line Coincidence Tables for Inductively Coupled 
Plasma Atomic Emission Spectrometry, 2nd edition. Pergamon Press, 
Oxford, United Kingdom, 1984.
9. Carcinogens--Working With Carcinogens, Department of Health, 
Education, and Welfare, Public Health Service, Center for Disease 
Control, National Institute for Occupational Safety and Health, 
Publication No. 77-206, Aug. 1977. Available from the National 
Technical Information Service (NTIS) as PB-277256.
10. OSHA Safety and Health Standards, General Industry, (29 CFR 1910), 
Occupational Safety and Health Administration, OSHA 2206, (Revised, 
January 1976).
11. Safety in Academic Chemistry Laboratories, American Chemical 
Society Publication, Committee on Chemical Safety, 3rd Edition, 1979.
12. Proposed OSHA Safety and Health Standards, Laboratories, 
Occupational Safety and Health Administration, Federal Register, July 
24, 1986.
13. Rohrbough, W.G. et al. Reagent Chemicals, American Chemical Society 
Specifications, 7th edition. American Chemical Society, Washington, DC, 
1986.
14. American Society for Testing and Materials. Standard Specification 
for Reagent Water, D1193-77. Annual Book of ASTM Standards, Vol. 11.01. 
Philadelphia, PA, 1991.
15. Code of Federal Regulations 40, Ch. 1, Pt. 136 Appendix B.
16. Maxfield, R. and B. Mindak. EPA Method Study 27, Method 200.7 Trace 
Metals by ICP, Nov. 1983. Available from National Technical Information 
Service (NTIS) as PB 85-248-656.
17. Botto, R.I. Quality Assurance in Operating a Multielement ICP 
Emission Spectrometer. Spectrochim. Acta, 39B(1):95-113, 1984.
18. Wallace, G.F., Some Factors Affecting the Performance of an ICP 
Sample Introduction System. Atomic Spectroscopy, Vol. 4, p. 188-192, 
1983.
19. Koirtyohann, S.R. et al. Nomenclature System for the Low-Power 
Argon Inductively Coupled Plasma, Anal. Chem. 52:1965, 1980.
20. Deming, S.N. and S.L. Morgan. Experimental Design for Quality and 
Productivity in Research, Development, and Manufacturing, Part III, pp. 
119-123. Short course publication by Statistical Designs, 9941 Rowlett, 
Suite 6, Houston, TX 77075, 1989.
21. Winefordner, J.D., Trace Analysis: Spectroscopic Methods for 
Elements, Chemical Analysis, Vol. 46, pp. 41-42.
22. Jones, C.L. et al. An Interlaboratory Study of Inductively Coupled 
Plasma Atomic Emission Spectroscopy Method 6010 and Digestion Method 
3050. EPA-600/4-87-032, U.S. Environmental Protection Agency, Las 
Vegas, Nevada, 1987.
23. Martin, T.D., E.R. Martin and SE. Long. Method 200.2: Sample 
Preparation Procedure for Spectrochemical Analyses of Total Recoverable 
Elements, EMSL ORD, USEPA, 1989.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 29825]]



            Table 1--Wavelengths, Estimated Instrument Detection Limits, and Recommended Calibration
----------------------------------------------------------------------------------------------------------------
                                                                                  Estimated
                                                              Wavelength\a\       detection     Calibrate\c\  to
                          Analyte                                 (nm)        limit\b\ ([mu]g/       (mg/L)
                                                                                     L)
----------------------------------------------------------------------------------------------------------------
Aluminum..................................................           308.215                45                10
Antimony..................................................           206.833                32                 5
Arsenic...................................................           193.759                53                10
Barium....................................................           493.409               2.3                 1
Beryllium.................................................           313.042              0.27                 1
Boron.....................................................           249.678               5.7                 1
Cadmium...................................................           226.502               3.4                 2
Calcium...................................................           315.887                30                10
Cerium....................................................           413.765                48                 2
Chromium..................................................           205.552               6.1                 5
Cobalt....................................................           228.616               7.0                 2
Copper....................................................           324.754               5.4                 2
Iron......................................................           259.940               6.2                10
Lead......................................................           220.353                42                10
Lithium...................................................           670.784           \d\ 3.7                 5
Magnesium.................................................           279.079                30                10
Manganese.................................................           257.610               1.4                 2
Mercury...................................................           194.227               2.5                 2
Molybdenum................................................           203.844                12                10
Nickel....................................................           231.604                15                 2
Phosphorus................................................           214.914                76                10
Potassium.................................................           766.491           \e\ 700                20
Selenium..................................................           196.090                75                 5
Silica (SiO2).............................................           251.611     \d\ 26 (SiO2)                10
Silver....................................................           328.068               7.0               0.5
Sodium....................................................           588.995                29                10
Strontium.................................................           421.552              0.77                 1
Thallium..................................................           190.864                40                 5
Tin.......................................................           189.980                25                 4
Titanium..................................................           334.941               3.8                10
Vanadium..................................................           292.402               7.5                 2
Zinc......................................................           213.856               1.8                 5
----------------------------------------------------------------------------------------------------------------
\a\ The wavelengths listed are recommended because of their sensitivity and overall acceptability. Other
  wavelengths may be substituted if they can provide the needed sensitivity and are treated with the same
  corrective techniques for spectral interference (see Section 4.1).
\b\ These estimated 3-sigma instrumental detection limits \16\ are provided only as a guide to instrumental
  limits. The method detection limits are sample dependent and may vary as the sample matrix varies. Detection
  limits for solids can be estimated by dividing these values by the grams extracted per liter, which depends
  upon the extraction procedure. Divide solution detection limits by 10 for 1 g extracted to 100 mL for solid
  detection limits.
\c\ Suggested concentration for instrument calibration.\2\ Other calibration limits in the linear ranges may be
  used.
\d\ Calculated from 2-sigma data.\5\
\e\ Highly dependent on operating conditions and plasma position.


[[Page 29826]]


   TABLE 2--On-Line Method Interelement Spectral Interferances Arising From Interferants at the 100 mg/L Level
----------------------------------------------------------------------------------------------------------------
                  Analyte                     Wavelength (nm)                     Interferant*
----------------------------------------------------------------------------------------------------------------
Ag.........................................           328.068  Ce, Ti, Mn
Al.........................................           308.215  V, Mo, Ce, Mn
As.........................................           193.759  V, Al, Co, Fe, Ni
B..........................................           249.678  None
Ba.........................................           493.409  None
Be.........................................           313.042  V, Ce
Ca.........................................           315.887  Co, Mo, Ce
Cd.........................................           226.502  Ni, Ti, Fe, Ce
Ce.........................................           413.765  None
Co.........................................           228.616  Ti, Ba, Cd, Ni, Cr, Mo, Ce
Cr.........................................           205.552  Be, Mo, Ni
Cu.........................................           324.754  Mo, Ti
Fe.........................................           259.940  None
Hg.........................................           194.227  V, Mo
K..........................................           766.491  None
Li.........................................           670.784  None
Mg.........................................           279.079  Ce
Mn.........................................           257.610  Ce
Mo.........................................           203.844  Ce
Na.........................................           588.995  None
Ni.........................................           231.604  Co, Tl
P..........................................           214.914  Cu, Mo
Pb.........................................           220.353  Co, Al, Ce, Cu, Ni, Ti, Fe
Sb.........................................           206.833  Cr, Mo, Sn, Ti, Ce, Fe
Se.........................................           196.099  Fe
SiO2.......................................           251.611  None
Sn.........................................           189.980  Mo, Ti, Fe, Mn, Si
Sr.........................................           421.552  None
Tl.........................................           190.864  Ti, Mo, Co, Ce, Al, V, Mn
Ti.........................................           334.941  None
V..........................................           292.402  Mo, Ti, Cr, Fe, Ce
Zn.........................................           213.856  Ni, Cu, Fe
----------------------------------------------------------------------------------------------------------------
* These on-line interferences from method analytes and titanium only were observed using an instrument with
  0.035 nm resolution (see Section 4.1.2). Interferant ranked by magnitude of intensity with the most severe
  interferant listed first in the row.


                                        TABLE 3--Mixed Standard Solutions
----------------------------------------------------------------------------------------------------------------
                 Solution                                                 Analytes
----------------------------------------------------------------------------------------------------------------
I.........................................  Ag, As, B, Ba, Ca, Cd, Cu, Mn, Sb, and Se
II........................................  K, Li, Mo, Na, Sr, and Ti
III.......................................  Co, P, V, and Ce
IV........................................  Al, Cr, Hg, SiO2, Sn, and Zn
V.........................................  Be, Fe, Mg, Ni, Pb, and Tl
----------------------------------------------------------------------------------------------------------------


        TABLE 4--Total Recoverable Method Detection Limits (MDL)
------------------------------------------------------------------------
                                  MDLs  Aqueous, mg/
             Analyte                    L\(1)\        Solids, mg/kg\(2)\
------------------------------------------------------------------------
Ag..............................               0.002                 0.3
Al..............................                0.02                   3
As..............................               0.008                   2
B...............................               0.003                  --
Ba..............................               0.001                 0.2
Be..............................              0.0003                 0.1
Ca..............................                0.01                   2
Cd..............................               0.001                 0.2
Ce..............................                0.02                   3
Co..............................               0.002                 0.4
Cr..............................               0.004                 0.8
Cu..............................               0.003                 0.5
Fe..............................               *0.03                   6
Hg..............................               0.007                   2
K...............................                 0.3                  60
Li..............................               0.001                 0.2
Mg..............................                0.02                   3
Mn..............................               0.001                 0.2
Mo..............................               0.004                   1

[[Page 29827]]

 
Na..............................                0.03                   6
Ni..............................               0.005                   1
P...............................                0.06                  12
Pb..............................                0.01                   2
Sb..............................               0.008                   2
Se..............................                0.02                   5
SiO2............................                0.02                  --
Sn..............................               0.007                   2
Sr..............................              0.0003                 0.1
Tl..............................               0.001                 0.2
Ti..............................                0.02                   3
V...............................               0.003                   1
Zn..............................               0.002                 0.3
------------------------------------------------------------------------
\(1)\ MDL concentrations are computed for original matrix with allowance
  for 2x sample preconcentration during preparation. Samples were
  processed in PTFE and diluted in 50-mL plastic centrifuge tubes.
\(2)\ Estimated, calculated from aqueous MDL determinations.
-- Boron not reported because of glassware contamination. Silica not
  determined in solid samples.
* Elevated value due to fume-hood contamination.


   TABLE 5--Inductively Coupled Plasma Instrument Operating Conditions
------------------------------------------------------------------------
 
------------------------------------------------------------------------
Incident rf power........................  1100 watts
Reflected rf power.......................  <5 watts
Viewing height above work coil...........  15 mm
Injector tube orifice i.d................  1 mm
Argon supply.............................  liquid argon
Argon pressure...........................  40 psi
Coolant argon flow rate..................  19 L/min.
Aerosol carrier argon flow rate..........  620 mL/min.
Auxiliary (plasma) argon flow rate.......  300 mL/min.
Sample uptake rate controlled to.........  1.2 mL/min.
------------------------------------------------------------------------


                                                Table 6--Precision and Recovery Data in Aqueous Matrices
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                 Average                                             Average
              Analyte                   Sample     Low spike   recovery  R     S (R)         RPD       High spike  recovery  R     S (R)         RPD
                                     conc.  mg/L      mg/L         (%)                                    mg/L         (%)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Tap Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           95          0.7          2.1          0.2           96          0.0          0.0
Al.................................        0.185         0.05           98          8.8          1.7          0.2          105          3.0          3.1
As.................................       <0.008         0.05          108          1.4          3.7          0.2          101          0.7          2.0
B..................................        0.023          0.1           98          0.2          0.0          0.4           98          0.2          0.5
Ba.................................        0.042         0.05          102          1.6          2.2          0.2           98          0.4          0.8
Be.................................      <0.0003         0.01          100          0.0          0.0          0.1           99          0.0          0.0
Ca.................................         35.2          5.0          101          8.8          1.7         20.0          103          2.0          0.9
Cd.................................       <0.001         0.01          105          3.5          9.5          0.1           98          0.0          0.0
Co.................................       <0.002         0.02          100          0.0          0.0          0.2           99          0.5          1.5
Cr.................................       <0.004         0.01          110          0.0          0.0          0.1          102          0.0          0.0
Cu.................................       <0.003         0.02          103          1.8          4.9          0.2          101          1.2          3.5
Fe.................................        0.008          0.1          106          1.0          1.8          0.4          105          0.3          0.5
Hg.................................       <0.007         0.05          103          0.7          1.9          0.2          100          0.4          1.0
K..................................         1.98          5.0          109          1.4          2.3          20.          107          0.7          1.7
Li.................................        0.006         0.02          103          6.9          3.8          0.2          110          1.9          4.4
Mg.................................         8.08          5.0          104          2.2          1.5         20.0          100          0.7          1.1
Mn.................................       <0.001         0.01          100          0.0          0.0          0.1           99          0.0          0.0
Mo.................................       <0.004         0.02           95          3.5         10.5          0.2          108          0.5          1.4
Na.................................         10.3          5.0           99          3.0          2.0         20.0          106          1.0          1.6
Ni.................................       <0.005         0.02          108          1.8          4.7          0.2          104          1.1          2.9
P..................................        0.045          0.1          102         13.1          9.4          0.4          104          3.2          1.3
Pb.................................        <0.01         0.05           95          0.7          2.1          0.2          100          0.2          0.5
Sb.................................       <0.008         0.05           99          0.7          2.0          0.2          102          0.7          2.0
Se.................................        <0.02          0.1           87          1.1          3.5          0.4           99          0.8          2.3
SiO2...............................          6.5          5.0          104          3.3          3.4         20.0           96          1.1          2.3
Sn.................................       <0.007         0.05          103          2.1          5.8          0.2          101          1.8          5.0
Sr.................................        0.181          0.1          102          3.3          2.1          0.4          105          0.8          1.0
Tl.................................        <0.02          0.1          101          3.9         10.9          0.4          101          0.1          0.3
V..................................       <0.003         0.05          101          0.7          2.0          0.2           99          0.2          0.5
Zn.................................        0.005         0.05          101          3.7          9.0          0.2           98          0.9          2.5
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                       Pond Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           92          0.0          0.0          0.2           94          0.0          0.0

[[Page 29828]]

 
Al.................................        0.819          0.2           88         10.0          5.0          0.8          100          2.9          3.7
As.................................       <0.008         0.05          102          0.0          0.0          0.2           98          1.4          4.1
B..................................        0.034          0.1          111          8.9          6.9          0.4          103          2.0          0.0
Ba.................................        0.029         0.05           96          0.9          0.0          0.2           97          0.3          0.5
Be.................................      <0.0003         0.01           95          0.4          1.1          0.2           95          0.0          0.0
Ca.................................         53.9          5.0            *            *          0.7         20.0          100          2.0          1.5
Cd.................................       <0.001         0.01          107          0.0          0.0          0.1           97          0.0          0.0
Co.................................       <0.002         0.02          100          2.7          7.5          0.2           97          0.7          2.1
Cr.................................       <0.004         0.01          105          3.5          9.5          0.1          103          1.1          2.9
Cu.................................       <0.003         0.02           98          2.1          4.4          0.2          100          0.5          1.5
Fe.................................        0.875          0.2           95          8.9          2.8          0.8           97          3.2          3.6
Hg.................................       <0.007         0.05           97          3.5         10.3          0.2           98          0.0          0.0
K..................................         2.48          5.0          106          0.3          0.1         20.0          103          0.2          0.4
Li.................................       <0.001         0.02          110          0.0          0.0          0.2          106          0.2          0.5
Mg.................................         10.8          5.0          102          0.5          0.0         20.0           96          0.7          1.3
Mn.................................        0.632         0.01            *            *          0.2          0.1           97          2.3          0.3
Mo.................................       <0.004         0.02          105          3.5          9.5          0.2          103          0.4          1.0
Na.................................         17.8          5.0          103          1.3          0.4         20.0           94          0.3          0.0
Ni.................................       <0.005         0.02           96          5.6          9.1          0.2          100          0.7          1.5
P..................................        0.196          0.1           91         14.7          0.3          0.4          108          3.9          1.3
Pb.................................        <0.01         0.05           96          2.6          7.8          0.2          100          0.7          2.0
Sb.................................       <0.008         0.05          102          2.8          7.8          0.2          104          0.4          1.0
Se.................................        <0.02          0.1          104          2.1          5.8          0.4          103          1.6          4.4
SiO2...............................         7.83          5.0          151          1.6          1.3         20.0          117          0.4          0.6
Sn.................................       <0.007         0.05           98          0.0          0.0          0.2           99          1.1          3.0
Sr.................................        0.129          0.1          105          0.4          0.0          0.4           99          0.1          0.2
Tl.................................        <0.02          0.1          103          1.1          2.9          0.4           97          1.3          3.9
V..................................        0.003         0.05           94          0.4          0.0          0.2           98          0.1          0.0
Zn.................................        0.006         0.05           97          1.6          1.8          0.2           94          0.4          0.0
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                       Well Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................       <0.002         0.05           97          0.7          2.1          0.2           96          0.2          0.5
Al.................................        0.036         0.05          107          7.6         10.1          0.2          101          1.1          0.8
As.................................       <0.008         0.05          107          0.7          1.9          0.2          104          0.4          1.0
B..................................        0.063          0.1           97          0.6          0.7          0.4           98          0.8          2.1
Ba.................................        0.102         0.05          102          3.0          0.0          0.2           99          0.9          1.0
Be.................................      <0.0003         0.01          100          0.0          0.0          0.1          100          0.0          0.0
Ca.................................         93.8          5.0            *            *          2.1         20.0          100          4.1          0.1
Cd.................................        0.002         0.01           90          0.0          0.0          0.1           96          0.0          0.0
Co.................................       <0.002         0.02           94          0.4          1.1          0.2           94          0.4          1.1
Cr.................................       <0.004         0.01          100          7.1         20.0          0.1          100          0.4          1.0
Cu.................................       <0.005         0.02          100          1.1          0.4          0.2           96          0.5          1.5
Fe.................................        0.042          0.1           99          2.3          1.4          0.4           97          1.4          3.3
Hg.................................       <0.007         0.05           94          2.8          8.5          0.2           93          1.2          3.8
K..................................         6.21          5.0           96          3.4          3.6         20.0          101          1.2          2.3
Li.................................        0.001         0.02          100          7.6          9.5          0.2          104          1.0          1.9
Mg.................................         24.5          5.0           95          5.6          0.3         20.0           93          1.6          1.2
Mn.................................         2.76         0.01            *            *          0.4          0.1            *            *          0.7
Mo.................................       <0.004         0.02          108          1.8          4.7          0.2          101          0.2          0.5
Na.................................         35.0          5.0          101         11.4          0.8         20.0          100          3.1          1.5
Ni.................................       <0.005         0.02          112          1.8          4.4          0.2           96          0.2          0.5
P..................................        0.197          0.1           95         12.7          1.9          0.4           98          3.4          0.9
Pb.................................        <0.01         0.05           87          4.9         16.1          0.2           95          0.2          0.5
Sb.................................       <0.008         0.05           98          2.8          8.2          0.2           99          1.4          4.0
Se.................................        <0.02          0.1          102          0.4          1.0          0.4           94          1.1          3.4
SiO2...............................         13.1          5.0           93          4.8          2.8         20.0           99          0.8          0.0
Sn.................................       <0.007         0.05           98          2.8          8.2          0.2           94          0.2          0.5
Sr.................................        0.274          0.1           94          5.7          2.7          0.4           95          1.7          2.2
Tl.................................        <0.02          0.1           92          0.4          1.1          0.4           95          1.1          3.2
V..................................       <0.003         0.05           98          0.0          0.0          0.2           99          0.4          1.0
Zn.................................        0.538         0.05            *            *          0.7          0.2           99          2.5          1.1
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                Sewage Treatment Effluent
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................        0.009         0.05           92          1.5          3.6          0.2           95          0.1          0.0
Al.................................         1.19         0.05            *            *          0.9          0.2          113         12.4          2.1
As.................................       <0.008         0.05           99          2.1          6.1          0.2           93          2.1          6.5
B..................................        0.226          0.1          217         16.3          9.5          0.4          119         13.1         20.9
Ba.................................        0.189         0.05           90          6.8          1.7          0.2           99          1.6          0.5

[[Page 29829]]

 
Be.................................      <0.0003         0.01           94          0.4          1.1          0.1          100          0.4          1.0
Ca.................................         87.9          5.0            *            *          0.6         20.0          101          3.7          0.0
Cd.................................        0.009         0.01           89          2.6          2.3          0.1           97          0.4          1.0
Co.................................        0.016         0.02           95          3.1          0.0          0.2           93          0.4          0.5
Cr.................................        0.128         0.01            *            *          1.5          0.1           97          2.4          2.7
Cu.................................        0.174         0.02           98         33.1          4.7          0.2           98          3.0          1.4
Fe.................................         1.28          0.1            *            *          2.8          0.4          111          7.0          0.6
Hg.................................       <0.007         0.05          102          1.4          3.9          0.2           98          0.5          1.5
K..................................         10.6          5.0          104          2.8          1.3         20.0          101          0.6          0.0
Li.................................        0.011         0.02          103          8.5          3.2          0.2          105          0.8          0.5
Mg.................................         22.7          5.0          100          4.4          0.0         20.0           92          1.1          0.2
Mn.................................        0.199         0.01            *            *          2.0          0.1          104          1.9          0.3
Mo.................................        0.125         0.02          110         21.2          6.8          0.2          102          1.3          0.9
Na.................................        0.236          5.0            *            *          0.0         20.0            *            *          0.4
Ni.................................        0.087         0.02          122         10.7          4.5          0.2           98          0.8          1.1
P..................................         4.71          0.1            *            *          2.6          0.4            *            *          1.4
Pb.................................        0.015         0.05           91          3.5          5.0          0.2           96          1.3          2.9
Sb.................................       <0.008         0.05           97          0.7          2.1          0.2          103          1.1          2.9
Se.................................        <0.02          0.1          108          3.9         10.0          0.4          101          2.6          7.2
SiO2...............................         16.7          5.0          124          4.0          0.9         20.0          108          1.1          0.8
Sn.................................        0.016         0.05           90          3.8          0.0          0.2           95          1.0          0.0
Sr.................................        0.515          0.1          103          6.4          0.5          0.4           96          1.6          0.2
Tl.................................        <0.02          0.1          105          0.4          1.0          0.4           95          0.0          0.0
V..................................        0.003         0.05           93          0.9          2.0          0.2           97          0.2          0.5
Zn.................................        0.160         0.05           98          3.3          1.9          0.2          101          1.0          1.4
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                   Industrial Effluent
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................      <0.0003         0.05           88          0.0          0.0          0.2           84          0.9          3.0
Al.................................        0.054         0.05           88         11.7         12.2          0.2           90          3.9          8.1
As.................................        <0.02         0.05           82          2.8          9.8          0.2           88          0.5          1.7
B..................................         0.17          0.1          162         17.6         13.9          0.4           92          4.7          9.3
Ba.................................        0.083         0.05           86          8.2          1.6          0.2           85          2.3          2.4
Be.................................      <0.0006         0.01           94          0.4          1.1          0.1           82          1.4          4.9
Ca.................................          500          5.0            *            *          2.8         20.0            *            *          2.3
Cd.................................        0.008         0.01           85          4.7          6.1          0.1           82          1.4          4.4
Co.................................       <0.004         0.02           93          1.8          5.4          0.2           83          0.4          1.2
Cr.................................        0.165         0.01            *            *          4.5          0.1          106          6.6          5.6
Cu.................................        0.095         0.02           93         23.3          0.9          0.2           95          2.7          2.8
Fe.................................        0.315          0.1           88         16.4          1.0          0.4           99          6.5          8.0
Hg.................................        <0.01         0.05           87          0.7          2.3          0.2           86          0.4          1.2
K..................................         2.87          5.0          101          3.4          2.4         20.0          100          0.8          0.4
Li.................................        0.069         0.02          103         24.7          5.6          0.2          104          2.5          2.2
Mg.................................         6.84          5.0           87          3.1          0.0         20.0           87          0.9          1.2
Mn.................................        0.141         0.01            *            *          1.2          0.1           89          6.6          4.8
Mo.................................         1.27         0.02            *            *          0.0          0.2          100         15.0          2.7
Na.................................         1500          5.0            *            *          2.7         20.0            *            *          2.0
Ni.................................        0.014         0.02           98          4.4          3.0          0.2           87          0.5          1.1
P..................................        0.326          0.1          105         16.0          4.7          0.4           97          3.9          1.4
Pb.................................        0.251         0.05           80         19.9          1.4          0.2           88          5.0          0.9
Sb.................................         2.81         0.05            *            *          0.4          0.2            *            *          2.0
Se.................................        0.021          0.1          106          2.6          3.2          0.4          105          1.9          4.6
SiO2...............................         6.83          5.0           99          6.8          1.7         20.0          100          2.2          3.0
Sn.................................        <0.01         0.05           87          0.7          2.3          0.2           86          0.4          1.2
Sr.................................         6.54          0.1            *            *          2.0          0.4            *            *          2.7
Tl.................................        <0.03          0.1           87          1.8          5.8          0.4           84          1.1          3.6
V..................................       <0.005         0.05           90          1.4          4.4          0.2           84          1.1          3.6
Zn.................................        0.024         0.05           89          6.0          4.4          0.2           91          3.5          8.9
--------------------------------------------------------------------------------------------------------------------------------------------------------
S (R) Standard deviation of percent recovery.
RPD Relative percent difference between duplicate spike determinations.
< Sample concentration below established method detection limit.
* Spike concentration <10% of sample background concentration.


[[Page 29830]]


                                                 Table 7--Precision and Recovery Data in Solid Matrices
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                        Sample                   Average                                             Average
              Analyte                 conc.  mg/  Low + spike   recovery R     S (R)         RPD         High +     recovery R     S (R)         RPD
                                          kg         mg/kg         (%)                                spike mg/kg      (%)
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                            EPA Hazardous Soil 884
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................          1.1           20           98          0.7          1.0          100           96          0.2          0.6
Al.................................         5080           20            *            *          7.2          100            *            *          5.4
As.................................          5.7           20           95          5.4         10.6          100           96          1.4          3.6
B..................................         20.4          100           93          2.7          5.3          400          100          2.1          5.5
Ba.................................          111           20           98         71.4         22.2          100           97         10.0          1.0
Be.................................         0.66           20           97          0.7          2.3          100           99          0.1          0.2
Ca.................................        85200            -            -            -            -            -            -            -            -
Cd.................................            2           20           93          0.7          1.0          100           94          0.2          0.4
Co.................................          5.5           20           96          3.5          7.7          100           93          0.8          2.1
Cr.................................         79.7           20           87         28.8         16.5          100          104          1.3          1.1
Cu.................................          113           20          110         16.2          4.4          100          104          4.0          4.2
Fe.................................        16500            -            -            -            -            -            -            -            -
Hg.................................         <1.4           10           92          2.5          7.7           40           98          0.0          0.0
K..................................          621          500          121          1.3          0.0         2000          107          0.9          1.8
Li.................................          6.7           10          113          3.5          4.4           40          106          0.6          0.6
Mg.................................        24400          500            *            *          8.4         2000            *            *         10.1
Mn.................................          343           20            *            *          8.5          100           95         11.0          1.6
Mo.................................          5.3           20           88          5.3         13.2          100           91          1.4          4.1
Na.................................          195          500          102          2.2          2.4         2000          100          1.5          3.7
Ni.................................         15.6           20          100          1.8          0.0          100           94          1.5          3.6
P..................................          595          500          106         13.4          8.0         2000          103          3.2          2.7
Pb.................................          145           20           88         51.8         17.9          100          108         15.6         17.4
Sb.................................          6.1           20           83          3.9          7.5          100           81          1.9          5.9
Se.................................           <5           20           79         14.7         52.4          100           99          0.7          2.1
Sn.................................         16.6           20           91         34.6          5.8           80          112          8.7          2.8
Sr.................................          102          100           84          9.6         10.8          400           94          2.5          4.6
Tl.................................           <4           20           92          4.8         14.6          100           91          1.5          4.6
V..................................         16.7           20          104          4.2          5.4          100           99          0.8          1.7
Zn.................................          131           20          103         31.2          7.3          100          104          7.2          6.4
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                        EPA Electroplating Sludge 286
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................            6           20           96          0.2          0.4          100           93          0.1          0.4
Al.................................         4980           20            *            *          4.4          100            *            *          5.6
As.................................           32           20           94          1.3          0.8          100           97          0.7          1.6
B..................................          210          100          113          2.0          1.6          400           98          1.9          3.5
Ba.................................         39.8           20            0          6.8          0.3          100            0          1.6          5.7
Be.................................         0.32           20           96          0.2          0.5          100          101          0.7          2.0
Ca.................................        48500            -            -            -            -            -            -            -            -
Cd.................................          108           20           98          2.5          0.8          100           96          0.5          0.5
Co.................................          5.9           20           93          2.9          5.7          100           93          0.6          1.5
Cr.................................         7580           20            *            *          0.7          100            *            *          1.3
Cu.................................          806           20            *            *          1.5          100           94          8.3          0.7
Fe.................................        31100            -            -            -            -            -            -            -            -
Hg.................................          6.1           10           90          2.5          4.0           40           97          1.7          4.3
K..................................         2390          500           75          8.3          4.0         2000           94          2.9          3.8
Li.................................          9.1           10          101          2.8          0.5           40          106          1.6          3.1
Mg.................................         1950          500          110          2.0          0.8         2000          108          2.3          3.2
Mn.................................          262           20            *            *          1.8          100           91          1.2          0.9
Mo.................................         13.2           20           92          2.1          2.9          100           92          0.3          0.0
Na.................................        73400          500            *            *          1.7         2000            *            *          1.4
Ni.................................          456           20            *            *          0.4          100           88          2.7          0.9
P..................................         9610          500            *            *          2.9         2000          114          7.4          3.4
Pb.................................         1420           20            *            *          2.1          100            *            *          1.3
Sb.................................           <2           20           76          0.9          3.3          100           75          2.8         10.7
Se.................................          6.3           20           86          9.0         16.6          100          103          1.6          2.7
Sn.................................         24.0           20           87          4.0          2.7           80           92          0.7          0.0
Sr.................................          145          100           90          8.1          8.1          400           93          2.4          4.6
Tl.................................           16           20           89          4.6          5.3          100           92          0.8          0.9
V..................................         21.7           20           95          1.2          1.0          100           96          0.4          0.9
Zn.................................        12500           20            *            *          0.8          100            *            *          0.8
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                 NBS 1645 River Sediment
--------------------------------------------------------------------------------------------------------------------------------------------------------
Ag.................................          1.6           20           92          0.4          1.0          100           96          0.3          0.9
Al.................................         5160           20            *            *          8.4          100            *            *          2.4
As.................................         62.8           20           89         14.4          9.7          100           97          2.9          5.0
B..................................         31.9          100          116          7.1         13.5          400           95          0.6          1.5
Ba.................................         54.8           20           95          6.1          2.8          100           98          1.2          1.3

[[Page 29831]]

 
Be.................................         0.72           20          101          0.4          1.0          100          103          1.4          3.9
Ca.................................        28000            -            -            -            -            -            -            -            -
Cd.................................          9.7           20          100          1.1          0.0          100          101          0.7          1.8
Co.................................          9.4           20           98          3.8          4.8          100           98          0.9          1.8
Cr.................................        28500           20            *            *          0.4          100            *            *          0.7
Cu.................................          109           20          115          8.5          0.0          100          102          1.8          1.0
Fe.................................        84800            -            -            -            -            -            -            -            -
Hg.................................          3.1           10           99          4.3          7.7           40           96          0.7          1.0
K..................................          452          500           98          4.1          2.0         2000          106          1.4          2.3
Li.................................          3.7           10          101          2.0          0.7           40          108          1.3          3.0
Mg.................................         6360          500            *            *          1.8         2000           93          2.7          1.0
Mn.................................          728           20            *            *          3.5          100           97         12.4          2.2
Mo.................................         17.9           20           97         12.5         18.5          100           98          0.6          0.0
Na.................................         1020          500           92          2.6          0.0         2000           97          1.1          1.7
Ni.................................         36.2           20           94          5.9          4.0          100          100          1.1          1.5
P..................................          553          500          102          1.4          0.9         2000          100          0.8          1.6
Pb.................................          707           20            *            *          0.8          100          103          5.9          0.4
Sb.................................         22.8           20           86          2.3          0.0          100           88          0.6          0.9
Se.................................          6.7           20          103         14.3         27.1          100           98          3.1          7.6
Sn.................................          309           20            *            *          1.0           80          101          7.9          2.7
Sr.................................          782          100           91         12.3          3.0          400           96          3.3          2.6
Tl.................................           <4           20           90          0.0          0.0          100           95          1.3          4.0
V..................................         20.1           20           89          5.4          5.8          100           98          0.7          0.0
Zn.................................         1640           20            *            *          1.8          100            *            *          1.1
--------------------------------------------------------------------------------------------------------------------------------------------------------
S (R) Standard deviation of percent recovery.
RPD Relative percent difference between duplicate spike determinations.
< Sample concentration below established method detection limit.
* Spike concentration <10% of sample background concentration.
- Not spiked.
+ Equivalent.


                  Table 8--ICP-AES Instrumental Precision and Accuracy for Aqueous Solutions a
----------------------------------------------------------------------------------------------------------------
                                          Mean conc.  (mg/                                       Accurace c  (%
                 Element                         L)                N b             RSD (%)         of Nominal)
----------------------------------------------------------------------------------------------------------------
Al......................................              14.8                 8               6.3               100
Sb......................................              15.1                 8               7.7               102
As......................................              14.7                 7               6.4                99
Ba......................................              3.66                 7               3.1                99
Be......................................              3.78                 8               5.8               102
Cd......................................              3.61                 8               7.0                97
Ca......................................              15.0                 8               7.4               101
Cr......................................              3.75                 8               8.2               101
Co......................................              3.52                 8               5.9                95
Cu......................................              3.58                 8               5.6                97
Fe......................................              14.8                 8               5.9               100
Pb......................................              14.4                 7               5.9                97
Mg......................................              14.1                 8               6.5                96
Mn......................................              3.70                 8               4.3               100
Mo......................................              3.70                 8               6.9               100
Ni......................................              3.70                 7               5.7               100
K.......................................              14.1                 8               6.6                95
Se......................................              15.3                 8               7.5               104
Na......................................              14.0                 8               4.2                95
Tl......................................              15.1                 7               8.5               102
V.......................................              3.51                 8               6.6                95
Zn......................................              3.57                 8               8.3               96
----------------------------------------------------------------------------------------------------------------
a These performance values are independent of sample preparation because the labs analyzed portions of the same
  solutions using sequential or simultaneous instruments.
b N = Number of measurements for mean and relative standard deviation (RSD).
c Accuracy is expressed as a percentage of the nominal value for each analyte in the acidified, multi-element
  solutions.


                            Table 9--Multilaboratory ICP Precision and Accuracy Data*
----------------------------------------------------------------------------------------------------------------
                                              Concentration
                  Analyte                        [mu]g/L              Total recoverable digestion [mu]/L
----------------------------------------------------------------------------------------------------------------
Aluminum...................................          69-4792  X = 0.9380 (C) + 22.1

[[Page 29832]]

 
                                             ...............  SR = 0.0481 (X) + 18.8
Antimony...................................          77-1406  0.8908 (C) + 0.9
                                             ...............  SR = 0.0682 (X) + 2.5
Arsenic....................................          69-1887  X = 1.0175 (C) + 3.9
                                             ...............  SR = 0.0643 (X) + 10.3
Barium.....................................            9-377  X = 0.8.80 (C) + 1.68
                                             ...............  SR = 0.0826 (X) + 3.54
Beryllium..................................           3-1906  X = 1.0177 (C) - 0.55
                                             ...............  SR = 0.0445 (X) - 0.10
Boron......................................          19-5189  X = 0.9676 (C) + 18.7
                                             ...............  SR = 0.0743 (X) + 21.1
Cadmium....................................           9-1943  X = 1.0137 (C) - 0.65
                                             ...............  SR = 0.0332 (X) + 0.90
Calcium....................................         17-47170  X = 0.9658 (C) + 0.8
                                             ...............  SR = 0.0327 (X) + 10.1
Chromium...................................          13-1406  X = 1.0049 (C) - 1.2
                                             ...............  SR = 0.0571 (X) + 1.0
Cobalt.....................................          17-2340  X = 0.9278 (C) + 1.5
                                             ...............  SR = 0.0407 (X) + 0.4
Copper.....................................           8-1887  X = 0.9647 (C) - 3.64
                                             ...............  SR = 0.0406 (X) + 0.96
Iron.......................................          13-9359  X = 0.9830 (C) + 5.7
                                             ...............  SR = 0.0790 (X) + 11.5
Lead.......................................          42-4717  X = 1.0056 (C) + 4.1
                                             ...............  SR = 0.0448 (X) + 3.5
Magnesium..................................         34-13868  X = 0.9879 (C) + 2.2
                                             ...............  SR = 0.0268 (X) + 8.1
Manganese..................................           4-1887  X = 0.9725 (C) + 0.07
                                             ...............  SR = 0.0400 (X) + 0.82
Molybdenum.................................          17-1830  X = 0.9707 (C) - 2.3
                                             ...............  SR = 0.0529 (X) + 2.1
Nickel.....................................         17-47170  X = 0.9869 (C) + 1.5
                                             ...............  SR = 0.0393 (X) + 2.2
Potassium..................................        347-14151  X = 0.9355 (C) - 183.1
                                             ...............  SR = 0.0329 (X) + 60.9
Selenium...................................          69-1415  X = 0.9737 (C) - 1.0
                                             ...............  SR = 0.0443 (X) + 6.6
Silicon....................................         189-9434  X = 0.9737 (C) - 22.6
                                             ...............  SR = 0.2133 (X) + 22.6
Silver.....................................            8-189  X = 0.3987 (C) + 8.25
                                             ...............  SR = 0.1836 (X) - 0.27
Sodium.....................................         35-47170  X = 1.0526 (C) + 26.7
                                             ...............  SR = 0.0884 (X) + 50.5
Thallium...................................          79-1434  X = 0.9238 (C) + 5.5
                                             ...............  SR = 0.0106 (X) + 48.0
Vanadium...................................          13-4698  X = 0.9551 (C) + 0.4
                                             ...............  SR = 0.0472 (X) + 0.5
Zinc.......................................           7-7076  X = 0.9500 (C) + 1.82
                                             ...............  SR = 0.0153 (X) + 7.78
----------------------------------------------------------------------------------------------------------------
\*\--Regression equations abstracted from Reference 16.
X = Mean Recovery, [mu]g/L.
C = True Value for the Concentration, [mu]g/L.
SR = Single-analyst Standard Deviation, [mu]g/L.

BILLING CODE 6560-50-P

[[Page 29833]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.007

BILLING CODE 6560-50-C

0
9. Revise Appendix D to Part 136 to read as follows:

Appendix D to Part 136--Precision and Recovery Statements for Methods 
for Measuring Metals

    Two selected methods from ``Methods for Chemical Analysis of 
Water and Wastes,'' EPA-600/4-79-020 (1979) have been subjected to 
interlaboratory method validation studies. The two selected methods 
are for Thallium and Zinc. The following precision and recovery 
statements are presented in this appendix and incorporated into Part 
136:

Method 279.2

    For Thallium, Method 279.2 (Atomic Absorption, Furnace 
Technique) replace the Precision and Accuracy Section statement with 
the following:

Precision and Accuracy

    An interlaboratory study on metal analyses by this method was 
conducted by the Quality Assurance Branch (QAB) of the

[[Page 29834]]

Environmental Monitoring Systems Laboratory--Cincinnati (EMSL-CI). 
Synthetic concentrates containing various levels of this element 
were added to reagent water, surface water, drinking water and three 
effluents. These samples were digested by the total digestion 
procedure, 4.1.3 in this manual. Results for the reagent water are 
given below. Results for other water types and study details are 
found in ``EPA Method Study 31, Trace Metals by Atomic Absorption 
(Furnace Techniques),'' National Technical Information Service, 5285 
Port Royal Road, Springfield, VA 22161 Order No. PB 86-121 704/AS, 
by Copeland, F.R. and Maney, J.P., January 1986.
    For a concentration range of 10.00-252 [micro]g[sol]L

X = 0.8781(C) - 0.715
S = 0.1112(X) + 0.669
SR = 0.1005(X) + 0.241

Where:

C = True Value for the Concentration, [micro]g/L
X = Mean Recovery, [micro]g/L
S = Multi-laboratory Standard Deviation, [micro]g/L
SR = Single-analyst Standard Deviation, [micro]g/L

Method 289.2

    For Zinc, Method 289.2 (Atomic Absorption, Furnace Technique) 
replace the Precision and Accuracy Section statement with the 
following:

Precision and Accuracy

    An interlaboratory study on metal analyses by this method was 
conducted by the Quality Assurance Branch (QAB) of the Environmental 
Monitoring Systems Laboratory--Cincinnati (EMSL-CI). Synthetic 
concentrates containing various levels of this element were added to 
reagent water, surface water, drinking water and three effluents. 
These samples were digested by the total digestion procedure, 4.1.3 
in this manual. Results for the reagent water are given below. 
Results for other water types and study details are found in ``EPA 
Method Study 31, Trace Metals by Atomic Absorption (Furnace 
Techniques),'' National Technical Information Service, 5285 Port 
Royal Road, Springfield, VA 22161 Order No. PB 86-121 704/AS, by 
Copeland, F.R. and Maney, J.P., January 1986.
    For a concentration range of 0.51-189 [micro]g[sol]L

X = 1.6710(C) + 1.485
S = 0.6740(X) - 0.342
SR = 0.3895(X)- 0.384

Where:

C = True Value for the Concentration, [micro]g[sol]L
X = Mean Recovery, [micro]g[sol]L
S = Multi-laboratory Standard Deviation, [micro]g[sol]L
SR = Single-analyst Standard Deviation, [micro]g[sol]L

PART 260--HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL

0
10. The authority citation for Part 260 continues to read as follows:

     Authority:  42 U.S.C. 6905, 6912(a), 6921-6927, 6930, 6934, 
6935, 6937, 6938, 6939, and 6974.

Subpart B--Definitions

0
11. Section 260.11 is amended by revising paragraph (c)(2) to read as 
follows:


Sec.  260.11  References.

* * * * *
    (c) * * *
    (2) Method 1664, n-Hexane Extractable Material (HEM; Oil and 
Grease) and Silica Gel Treated n-Hexane Extractable Material SGT-HEM; 
Non-polar Material) by Extraction and Gravimetry:
    (i) Revision A, EPA-821-R-98-002, February 1999, IBR approved for 
Part 261, Appendix IX.
    (ii) Revision B, EPA-821-R-10-001, February 2010, IBR approved for 
Part 261, Appendix IX.
* * * * *

PART 423--STEAM ELECTRIC POWER GENERATING POINT SOURCE CATEGORY

0
12. The authority citation for Part 423 continues to read as follows:

    Authority:  Secs. 301; 304(b), (c), (e), and (g); 306(b) and 
(c); 307(b) and (c); and 501, Clean Water Act (Federal Water 
Pollution Control Act Amendments of 1972, as amended by Clean Water 
Act of 1977) (the ``Act''; 33 U.S.C. 1311; 1314(b), (c), (e), and 
(g); 1316(b) and (c); 1317(b) and (c); and 1361; 86 Stat. 816, Pub. 
L. 92-500; 91 Stat. 1567, Pub. L. 95-217), unless otherwise noted.


0
13. Section 423.11 is amended by revising paragraphs (a) and (l) to 
read as follows:


Sec.  423.11  Specialized definitions.

* * * * *
    (a) The term total residual chlorine (or total residual oxidants 
for intake water with bromides) means the value obtained using any of 
the ``chlorine--total residual'' methods in Table IB in 40 CFR 
136.3(a), or other methods approved by the permitting authority.
* * * * *
    (l) The term free available chlorine means the value obtained using 
any of the ``chlorine--free available'' methods in Table IB in 40 CFR 
136.3(a) where the method has the capability of measuring free 
available chlorine, or other methods approved by the permitting 
authority.
* * * * *

PART 430--PULP, PAPER, AND PAPERBOARD POINT SOURCE CATEGORY

0
14. The authority citation for Part 430 continues to read as follows:

    Authority: Secs. 301, 304, 306, 307, 308, 402, and 501, Clean 
Water Act as amended, (33 U.S.C. 1311, 1314, 1316, 1317, 1318, 1342, 
and 1361) and Section 112 of the Clean Air Act, as amended (42 
U.S.C. 7412).


0
15. Section 430.01 is amended by revising paragraph (a) and by adding 
paragraphs (s) through (v) to read as follows:


Sec.  430.01  General definitions.

* * * * *
    (a) Adsorbable organic halides (AOX). A bulk parameter that 
measures the total mass of chlorinated organic matter in water and 
wastewater. The approved method of analysis for AOX is Method 1650, 
which is available in Appendix A of this part, and online at http://water.epa.gov/scitech/methods/cwa/index.cfm.
* * * * *
    (s) TCDD. 2,3,7,8-tetrachlorodibenzo-p-dioxin. The approved method 
of analysis for TCDD is Method 1613B, which is available in Appendix A 
of this part, and online at http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (t) TCDF. 2,3,7,8-tetrachlorodibenzofuran. The approved method of 
analysis for TCDF is Method 1613B, which is available in Appendix A of 
this part, and online at http://water.epa.gov/scitech/methods/cwa/index.cfm.
    (u) Chloroform. The approved methods of analysis for chloroform are 
listed in Table IC at 40 CFR 136.3.
    (v) The approved method of analysis for the following chlorinated 
phenolic compounds is Method 1653, which is available in Appendix A of 
this part, and online at http://water.epa.gov/scitech/methods/cwa/index.cfm:
    (1) Trichlorosyringol.
    (2) 3,4,5-Trichlorocatechol.
    (3) 3,4,6-Trichlorocatechol.
    (4) 3,4,5-Trichloroguaiacol.
    (5) 3,4,6-Trichloroguaiacol.
    (6) 4,5,6-Trichloroguaiacol.
    (7) 2,4,5-Trichlorophenol.
    (8) 2,4,6-Trichlorophenol.
    (9) Tetrachlorocatechol.
    (10) Tetrachloroguaiacol.
    (11) 2,3,4,6-Tetrachlorophenol.
    (12) Pentachlorophenol.

PART 435--OIL AND GAS EXTRACTION POINT SOURCE CATEGORY

0
16. The authority citation for part 435 continues to read as follows:

    Authority: 33 U.S.C. 1311, 1314, 1316, 1317, 1318, 1342, and 
1361.

0
17. Section 435.11 is amended as follows:
0
a. By revising paragraph (d).
0
b. By revising paragraph (e).
0
c. By revising paragraph (k)(2).

[[Page 29835]]

0
d. By revising paragraph (o).
0
e. By revising paragraph (t).
0
f. By revising paragraph (u).
0
g. By revising paragraph (v).
0
h. By revising paragraph (x).
0
i. By revising paragraph (ee).
0
j. By revising paragraph (gg).
0
k. By revising paragraph (hh).
0
l. By revising paragraph (ss).
0
m. By adding paragraph (uu).


Sec.  435.11  Special definitions.

* * * * *
    (d) Base fluid retained on cuttings as applied to BAT effluent 
limitations and NSPS refers to the ``Determination of the Amount of 
Non-Aqueous Drilling Fluid (NAF) Base Fluid from Drill Cuttings by a 
Retort Chamber (Derived from API Recommended Practice 13B-2)'', EPA 
Method 1674, which is published as an appendix to Subpart A of this 
part and in ``Analytic Methods for the Oil and Gas Extraction Point 
Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this 
section.
    (e) Biodegradation rate as applied to BAT effluent limitations and 
NSPS for drilling fluids and drill cuttings refers to the ``Protocol 
for the Determination of Degradation of Non Aqueous Base Fluids in a 
Marine Closed Bottle Biodegradation Test System: Modified ISO 
11734:1995,'' EPA Method 1647, supplemented with ``Procedure for Mixing 
Base Fluids With Sediments,'' EPA Method 1646. Both EPA Method 1646 and 
1647 are published as appendices to Subpart A of this part and in 
``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See paragraph (uu) of this section.
* * * * *
    (k) * * *
    (2) Dry drill cuttings means the residue remaining in the retort 
vessel after completing the retort procedure specified in EPA Method 
1674, which is published as an appendix to Subpart A of this part and 
in ``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See paragraph (uu) of this section.
* * * * *
    (o) Formation oil means the oil from a producing formation which is 
detected in the drilling fluid, as determined by the GC/MS compliance 
assurance method, EPA Method 1655, when the drilling fluid is analyzed 
before being shipped offshore, and as determined by the RPE method, EPA 
Method 1670, when the drilling fluid is analyzed at the offshore point 
of discharge. The GC/MS compliance assurance method and the RPE method 
approved for use with this part are published as appendices to Subpart 
A of this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this 
section. Detection of formation oil by the RPE method may be confirmed 
by the GC/MS compliance assurance method, and the results of the GC/MS 
compliance assurance method shall apply instead of those of the RPE 
method.
* * * * *
    (t) Maximum weighted mass ratio averaged over all NAF well sections 
for BAT effluent limitations and NSPS for base fluid retained on 
cuttings means the weighted average base fluid retention for all NAF 
well sections as determined by EPA Method 1674, which is published as 
an appendix to Subpart A of this part and in ``Analytic Methods for the 
Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See 
paragraph (uu) of this section.
    (u) Method 1654A refers to EPA Method 1654, Revision A, entitled 
``PAH Content of Oil by HPLC/UV,'' December 1992, which is published as 
an appendix to Subpart A of this part and in ``Analytic Methods for the 
Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-004. See 
paragraph (uu) of this section.
    (v) Minimum as applied to BAT effluent limitations and NSPS for 
drilling fluids and drill cuttings means the minimum 96-hour 
LC50 value allowed as measured in any single sample of the 
discharged waste stream. Minimum as applied to BPT and BCT effluent 
limitations and NSPS for sanitary wastes means the minimum 
concentration value allowed as measured in any single sample of the 
discharged waste stream.
* * * * *
    (x) No discharge of free oil means that waste streams may not be 
discharged that contain free oil as evidenced by the monitoring method 
specified for that particular stream, e.g., deck drainage or 
miscellaneous discharges cannot be discharged when they would cause a 
film or sheen upon or discoloration of the surface of the receiving 
water; drilling fluids or cuttings may not be discharged when they fail 
EPA Method 1617 (Static Sheen Test), which is published as an appendix 
to Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph 
(uu) of this section.
* * * * *
    (ee) Sediment toxicity as applied to BAT effluent limitations and 
NSPS for drilling fluids and drill cuttings refers to EPA Method 1644: 
``Method for Conducting a Sediment Toxicity Test with Leptocheirus 
plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based Drilling 
Muds'' and sediment preparation procedures specified in EPA Method 
1646. EPA Method 1644 is published in ``Analytic Methods for the Oil 
and Gas Extraction Point Source Category,'' (see paragraph (uu) of this 
section) and EPA Method 1646 is published as an appendix to Subpart A 
of this part.
* * * * *
    (gg) SPP toxicity as applied to BAT effluent limitations and NSPS 
for drilling fluids and drill cuttings refers to the bioassay test 
procedure, ``Suspended Particulate Phase (SPP) Toxicity Test,'' 
presented in EPA Method 1619, which is published as an appendix to 
Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph 
(uu) of this section.
    (hh) Static sheen test means the standard test procedure that has 
been developed for this industrial subcategory for the purpose of 
demonstrating compliance with the requirement of no discharge of free 
oil. The methodology for performing the static sheen test is presented 
in EPA Method 1617, which is published as an appendix to Subpart A of 
this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See paragraph (uu) of this 
section.
* * * * *
    (ss) C16-C18 internal olefin drilling fluid 
means a C16-C18 internal olefin drilling fluid 
formulated as specified in appendix 1 of subpart A of this part.
* * * * *
    (uu) Analytic Methods for the Oil and Gas Extraction Point Source 
Category is the EPA document, ``Analytic Methods for the Oil and Gas 
Point Source Category,'' December 2011, EPA-821-R-11-004, that compiles 
analytic methods for this category. This incorporation by reference was 
approved by the Director of the Federal Register in accordance with 5 
U.S.C. 552(a) and 1 CFR part 51. Copies may be inspected at the 
National Archives and Records Administration (NARA). For information on 
the availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be inspected at EPA's 
Water Docket, 1200 Pennsylvania Ave. NW., Washington, DC 20460. This 
method may be obtained

[[Page 29836]]

at http://water.epa.gov/scitech/methods/cwa/index.cfm.

0
18. In Sec.  435.12, Footnote 1 to the table is revised to read as 
follows:


Sec.  435.12  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
practicable control technology currently available (BPT).

* * * * *
    \1\ No discharge of free oil. See Sec.  435.11(x).
* * * * *

0
19. In Sec.  435.13:
0
a. Remove ``LC5'' and add in its place ``LC50'' 
wherever it appears.
0
b. Footnotes 2, 3, and 5 through 11 to the table are revised to read as 
follows:


Sec.  435.13  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
available technology economically achievable (BAT).

* * * * *
    \2\ As determined by the suspended particulate phase (SPP) 
toxicity test. See Sec.  435.11(gg).
    \3\ As determined by the static sheen test. See Sec.  
435.11(hh).
* * * * *
    \5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) 
of stock base fluid as determined by EPA Method 1654, Revision A, 
[specified at Sec.  435.11(u)] entitled ``PAH Content of Oil by 
HPLC/UV,'' December 1992, which is published as an appendix to 
Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See Sec.  
435.11(uu).
    \6\ Base fluid sediment toxicity ratio = 10-day LC50 
of C16-C18 internal olefin/10-day 
LC50 of stock base fluid as determined by EPA Method 
1644: ``Method for Conducting a Sediment Toxicity Test with 
Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or 
Synthetic-Based Drilling Muds'' after preparing the sediment 
according to the procedure specified in EPA Method 1646, which are 
published as appendices to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(ee) and (uu).
    \7\ Biodegradation rate ratio = Cumulative headspace gas 
production (ml) of C16-C18 internal olefin/
Cumulative headspace gas production (ml) of stock base fluid, both 
at 275 days as determined by EPA Method 1647, which is published as 
an appendix to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(e) and (uu).
    \8\ Drilling fluid sediment toxicity ratio = 4-day 
LC50 of C16-C18 internal olefin 
drilling fluid/4-day LC50 of drilling fluid removed from 
drill cuttings at the solids control equipment as determined by EPA 
Method 1644: ``Method for Conducting a Sediment Toxicity Test with 
Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or 
Synthetic-Based Drilling Muds'' after sediment preparation 
procedures specified in EPA Method 1646, which are published as 
appendices to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(ee) and (uu).
    \9\ As determined before drilling fluids are shipped offshore by 
the GC/MS compliance assurance method (EPA Method 1655), and as 
determined prior to discharge by the RPE method (EPA Method 1670) 
applied to drilling fluid removed from drill cuttings. If the 
operator wishes to confirm the results of the RPE method (EPA Method 
1670), the operator may use the GC/MS compliance assurance method 
(EPA Method 1655). Results from the GC/MS compliance assurance 
method (EPA Method 1655) shall supersede the results of the RPE 
method (EPA Method 1670). EPA Method 1655 and 1670 are published as 
appendices to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(uu).
    \10\ Maximum permissible retention of non-aqueous drilling fluid 
(NAF) base fluid on wet drill cuttings averaged over drilling 
intervals using NAFs as determined by EPA Method 1674, which is 
published as an appendix to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(uu). This limitation is applicable 
for NAF base fluids that meet the base fluid sediment toxicity ratio 
(Footnote 6), biodegradation rate ratio (Footnote 7), PAH, mercury, 
and cadmium stock limitations (C16-C18 
internal olefin) defined above in this table.
    \11\ Maximum permissible retention of non-aqueous drilling fluid 
(NAF) base fluid on wet drill cuttings average over drilling 
intervals using NAFs as determined by EPA Method 1674, which is 
published as an appendix to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(uu). This limitation is applicable 
for NAF base fluids that meet the ester base fluid sediment toxicity 
ratio and ester biodegradation rate ratio stock limitations defined 
as:
    (a) ester base fluid sediment toxicity ratio = 10-day 
LC50 of C12-C14 ester or 
C8 ester/10-day LC50 of stock base fluid as 
determined by EPA Method 1644: ``Method for Conducting a Sediment 
Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling 
Fluids or Synthetic-Based Drilling Muds'' after sediment preparation 
procedures specified in EPA Method 1646, which are published as 
appendices to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(ee) and (uu);
    (b) ester biodegradation rate ratio = Cumulative headspace gas 
production (ml) of C12-C14 ester or 
C8 ester/Cumulative headspace gas production (ml) of 
stock base fluid, both at 275 days as determined by EPA Method 1647, 
which is published as an appendix to Subpart A of this part and in 
``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See Sec.  435.11(e) and (uu); and
    (c) PAH mass ratio (Footnote 5), mercury, and cadmium stock 
limitations (C16-C18 internal olefin) defined 
above in this table.

0
20. In Sec.  435.14 footnote 2 to the table is revised to read as 
follows:


Sec.  435.14  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
conventional pollutant control technology (BCT).

* * * * *
    \2\ As determined by the static sheen test. See Sec.  
435.11(hh).
* * * * *

0
21. In Sec.  435.15:
0
a. Remove ``LC5'' and add in its place 
``LC50''wherever it appears.
0
b. Footnotes 2, 3, and 5 through 11 to the table are revised to read as 
follows:


Sec.  435.15  Standards of performance for new sources (NSPS).

* * * * *
    \2\ As determined by the suspended particulate phase (SPP) 
toxicity test. See Sec.  435.11(gg).
    \3\ As determined by the static sheen test. See Sec.  
435.11(hh).
* * * * *
    \5\ PAH mass ratio = Mass (g) of PAH (as phenanthrene)/Mass (g) 
of stock base fluid as determined by EPA Method 1654, Revision A, 
[specified at Sec.  435.11(u)] entitled ``PAH Content of Oil by 
HPLC/UV,'' December 1992, which is published as an appendix to 
Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See Sec.  
435.11(uu).
    \6\ Base fluid sediment toxicity ratio = 10-day LC50 
of C16-C18 internal olefin/10-day 
LC50 of stock base fluid as determined by EPA Method 
1644: ``Method for Conducting a Sediment Toxicity Test with 
Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or 
Synthetic-Based Drilling Muds'' after preparing the sediment 
according to the procedure specified in EPA Method 1646, which are 
published as appendices to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(ee) and (uu).
    \7\ Biodegradation rate ratio = Cumulative headspace gas 
production (ml) of C16-C18 internal olefin/
Cumulative headspace gas production (ml) of stock base fluid, both 
at 275 days as determined by EPA Method 1647, which is published as 
an appendix to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(e) and (uu).
    \8\ Drilling fluid sediment toxicity ratio = 4[dash]day 
LC50 of C16-C18 internal olefin 
drilling fluid/4-day LC50 of drilling fluid removed from 
drill cuttings at the solids control equipment as determined by EPA 
Method 1644: ``Method for Conducting a Sediment Toxicity Test with 
Leptocheirus plumulosus and Non-Aqueous Drilling Fluids or 
Synthetic-Based Drilling Muds'' after sediment preparation 
procedures specified in

[[Page 29837]]

EPA Method 1646, which are published as appendices to Subpart A of 
this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See Sec.  435.11(ee) and 
(uu).
    \9\ As determined before drilling fluids are shipped offshore by 
the GC/MS compliance assurance method (EPA Method 1655), and as 
determined prior to discharge by the RPE method (EPA Method 1670) 
applied to drilling fluid removed from drill cuttings. If the 
operator wishes to confirm the results of the RPE method (EPA Method 
1670), the operator may use the GC/MS compliance assurance method 
(EPA Method 1655). Results from the GC/MS compliance assurance 
method (EPA Method 1655) shall supersede the results of the RPE 
method (EPA Method 1670). EPA Method 1655 and 1670 are published as 
appendices to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(uu).
    \10\ Maximum permissible retention of non-aqueous drilling fluid 
(NAF) base fluid on wet drill cuttings averaged over drilling 
intervals using NAFs as determined by EPA Method 1674, which is 
published as an appendix to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(uu). This limitation is applicable 
for NAF base fluids that meet the base fluid sediment toxicity ratio 
(Footnote 6), biodegradation rate ratio (Footnote 7), PAH, mercury, 
and cadmium stock limitations (C16-C18 
internal olefin) defined above in this table.
    \11\ Maximum permissible retention of non-aqueous drilling fluid 
(NAF) base fluid on wet drill cuttings average over drilling 
intervals using NAFs as determined by EPA Method 1674, which is 
published as an appendix to Subpart A of this part and in ``Analytic 
Methods for the Oil and Gas Extraction Point Source Category,'' EPA-
821-R-11-004. See Sec.  435.11(uu). This limitation is applicable 
for NAF base fluids that meet the ester base fluid sediment toxicity 
ratio and ester biodegradation rate ratio stock limitations defined 
as:
    (a) ester base fluid sediment toxicity ratio = 10-day 
LC50 of C12-C14 ester or 
C8 ester/10-day LC50 of stock base fluid as 
determined by EPA Method 1644: ``Method for Conducting a Sediment 
Toxicity Test with Leptocheirus plumulosus and Non-Aqueous Drilling 
Fluids or Synthetic-Based Drilling Muds'' after sediment preparation 
procedures specified in EPA Method 1646, which are published as 
appendices to Subpart A of this part and in ``Analytic Methods for 
the Oil and Gas Extraction Point Source Category,'' EPA-821-R-11-
004. See Sec.  435.11(ee) and (uu);
    (b) ester biodegradation rate ratio = Cumulative headspace gas 
production (ml) of C12-C14 ester or 
C8 ester/Cumulative headspace gas production (ml) of 
stock base fluid, both at 275 days as determined by EPA Method 1647, 
which is published as an appendix to Subpart A of this part and in 
``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See Sec.  435.11(e) and (uu); and (c) 
PAH mass ratio (Footnote 5), mercury, and cadmium stock limitations 
(C16-C18 internal olefin) defined above in 
this table.

0
22. The heading of Appendix 1 to Subpart A of Part 435 is revised to 
read as follows:

Appendix 1 to Subpart A of Part 435-- Static Sheen Test (EPA Method 
1617)

* * * * *

0
23. Appendix 2 to Subpart A of Part 435 is amended as follows:
0
a. Revise the appendix heading.
0
b. Remove the fourth sentence from Section II.C.6.
0
c. Revise Section III.A.1.
0
d. Revise Section III.E.2.
    The revisions read as follows:

Appendix 2 to Subpart A of Part 435--Drilling Fluids Toxicity Test (EPA 
Method 1619)

* * * * *
III-A. * * *

    (1) Each definitive test consists of 18 test containers: 3 
replicates of a control and 5 SPP dilutions. Test containers should 
be Pyrex or equivalent glass. For definitive tests, 5 SPP dilutions 
with 3 replicates of at least 500 ml each are required. Twenty 
mysids per replicate, 360 per definitive test are required.
* * * * *
III-E. * * *
    (2) Establish the definitive test concentrations based on 
results of a range finding test or based on prior experience and 
knowledge of the mud system.
* * * * *

0
24. The heading of Appendix 3 to Subpart A of Part 435 is amended to 
read as follows:

Appendix 3 to Subpart A of Part 435--Procedure for Mixing Base Fluids 
With Sediments (EPA Method 1646)

* * * * *

0
25. Appendix 4 to Subpart A of Part 435 is revised to read as follows:

Appendix 4 to Subpart A of Part 435-- Protocol for the Determination of 
Degradation of Non-Aqueous Base Fluids in a Marine Closed Bottle 
Biodegradation Test System: Modified ISO 11734:1995 (EPA Method 1647)

1.0. Summary of EPA Method 1647

    a. This method determines the anaerobic degradation potential of 
mineral oils, paraffin oils and non-aqueous fluids (NAF) in 
sediments. These substrates are base fluids for formulating offshore 
drilling fluids. The test evaluates base fluid biodegradation rates 
by monitoring gas production due to microbial degradation of the 
test fluid in natural marine sediment.
    b. The test procedure places a mixture of marine/estuarine 
sediment, test substrate (hydrocarbon or controls) and seawater into 
clean 120 mL (150 mL actual volume) Wheaton serum bottles. The test 
is run using four replicate serum bottles containing 2,000 mg 
carbon/kg dry weight concentration of test substrate in sediment. 
The use of resazurin dye solution (1 ppm) evaluates the anaerobic 
(redox) condition of the bottles (dye is blue when oxygen is 
present, reddish in low oxygen conditions and colorless if oxygen 
free). After capping the bottles, a nitrogen sparge removes air in 
the headspace before incubation begins. During the incubation 
period, the sample should be kept at a constant temperature of 29 
 1[deg]C. Gas production and composition is measured 
approximately every two weeks. The samples need to be brought to 
ambient temperature before making the measurements. Measure gas 
production using a pressure gauge. Barometric pressure is measured 
at the time of testing to make necessary volume adjustments.
    c. ISO 11734:1995 specifies that total gas is the standard 
measure of biodegradation. While modifying this test for evaluating 
biodegradation of NAFs, methane was also monitored and found to be 
an acceptable method of evaluating biodegradation. Section 7 
contains the procedures used to follow biodegradation by methane 
production. Measurement of either total gas or methane production is 
permitted. If methane is followed, determine the composition of the 
gas by using gas chromatography (GC) analysis at each sampling. At 
the end of the test when gas production stops, or at around 275 
days, an analysis of sediment for substrate content is possible. 
Common methods which have been successfully used for analyzing NAFs 
from sediments are listed in Section 8.

2.0 System Requirements

    This environmental test system has three phases, spiked 
sediment, overlying seawater, and a gas headspace. The sediment/test 
compound mixture is combined with synthetic sea water and 
transferred into 120-mL serum bottles. The total volume of sediment/
sea water mixture in the bottles is 75 mL. The volume of the 
sediment layer will be approximately 50 mL, but the exact volume of 
the sediment will depend on sediment characteristics (wet:dry ratio 
and density). The amount of synthetic sea water will be calculated 
to bring the total volume in the bottles to 75 mL. The test systems 
are maintained at a temperature of 29  1[deg]C during 
incubation. The test systems are brought to ambient temperatures 
prior to measuring pressure or gas volume.

2.1 Sample Requirements

    a. The concentration of base fluids are at least 2,000 mg carbon 
test material/kg dry sediment. Carbon concentration is determined by 
theoretical composition based on the chemical formula or by chemical 
analysis by ASTM D5291-96. Sediments with positive, intermediate and 
negative control substances as well as a C16-
C18 internal olefin type base fluid will be run in 
conjunction with test materials under the same conditions. The 
positive control is ethyl oleate (CAS 111-62-6), the intermediate 
control is 1-hexadecene (CAS 629-73-2), and the negative control is 
squalane (CAS 111-01-3). Controls must be of analytical grade or

[[Page 29838]]

the highest grade available. Each test control concentration should 
be prepared according to the mixing procedure described in Section 
3.1.
    b. Product names will be used for examples or clarification in 
the following text. Any use of trade or product names in this 
publication is for descriptive use only, and does not constitute 
endorsement by EPA or the authors.

2.2. Seawater Requirements

    Synthetic seawater at a salinity of 25  1 ppt should 
be used for the test. The synthetic seawater should be prepared by 
mixing a commercially available artificial seawater mix, into high 
purity distilled or de-ionized water. The seawater should be aerated 
and allowed to age for approximately one month prior to use.

2.3. Sediment Requirements

    a. The dilution sediment must be from a natural estuarine or 
marine environment and be free of the compounds of interest. The 
collection location, date and time will be documented and reported. 
The sediment is prepared by press-sieving through a 2,000-micron 
mesh sieve to remove large debris, then press-sieving through a 500-
micron sieve to remove indigenous organisms that may confound test 
results. The water content of the sediment should be less than 60% 
(w/w) or a wet to dry ratio of 2.5. The sediment should have a 
minimum organic matter content of 3% (w/w) as determined by ASTM 
D2974-07a (Method A and D and calculate organic matter as in Section 
8.3 of method ASTM D2974-07a).
    b. To reduce the osmotic shock to the microorganisms in the 
sediment the salinity of the sediment's pore water should be between 
20-30 ppt. Sediment should be used for testing as soon as possible 
after field collection. If required, sediment can be stored in the 
dark at 4 [deg]C with 3-6 inches of overlying water in a sealed 
container for a maximum period of 2 months prior to use.

3.0 Test Set Up

    The test is set up by first mixing the test or control 
substrates into the sediment inoculum, then mixing in seawater to 
make a pourable slurry. The slurry is then poured into serum 
bottles, which are then flushed with nitrogen and sealed.

3.1. Mixing Procedure

    Because base fluids are strongly hydrophobic and do not readily 
mix with sediments, care must be taken to ensure base fluids are 
thoroughly homogenized within the sediment. All concentrations are 
weight-to-weight comparisons (mg of base fluid to kg of dry control 
sediment). Sediment and base fluid mixing will be accomplished by 
using the following method.
    3.1.1. Determine the wet to dry weight ratio for the control 
sediment by weighing approximately 10 sub-samples of approximately 1 
g each of the screened and homogenized wet sediment into tared 
aluminum weigh pans. Dry sediment at 105 [deg]C for 18-24 h. Remove 
the dried sediments and cool in a desiccator. Repeat the drying, 
cooling, and weighing cycle until a constant weight is achieved 
(within 4% of previous weight). Re-weigh the samples to determine 
the dry weight. Calculate the mean wet and dry weights of the 10 sub 
samples and determine the wet/dry ratio by dividing the mean wet 
weight by the mean dry weight using Equation 5-1. This is required 
to determine the weight of wet sediment needed to prepare the test 
samples.
[GRAPHIC] [TIFF OMITTED] TR18MY12.008

    3.1.2. Determine the density (g/ml) of the wet sediment. This 
will be used to determine total volume of wet sediment needed for 
the various test treatments. One method is to tare a 5 ml graduated 
cylinder and add about 5 ml of homogenized sediment. Carefully 
record the volume then weigh this volume of sediment. Repeat this a 
total of three times. To determine the wet sediment density, divide 
the weight by volume per the following formula:
[GRAPHIC] [TIFF OMITTED] TR18MY12.009

    3.1.3. Determine the amount of base fluid to be spiked into wet 
sediment in order to obtain the desired initial base fluid 
concentration of 2,000 mg carbon/kg dry weight. An amount of wet 
sediment that is the equivalent of 30 g of dry sediment will be 
added to each bottle. A typical procedure is to prepare enough 
sediment for 8 serum bottles (3 bottles to be sacrificed at the 
start of the test, 4 bottles incubated for headspace analysis, and 
enough extra sediment for 2 extra bottles). Extra sediment is needed 
because some of the sediment will remain coated onto the mixing bowl 
and utensils. Experience with this test may indicate that preparing 
larger volumes of spiked sediment is a useful practice, then the 
following calculations should be adjusted accordingly.
    a. Determine the total weight of dry sediment needed to add 30 g 
dry sediment to 8 bottles. If more bottles are used then the 
calculations should be modified accordingly. For example:
[GRAPHIC] [TIFF OMITTED] TR18MY12.010

    b. Determine the weight of base fluid, in terms of carbon, 
needed to obtain a final base fluid concentration of 2,000 mg 
carbon/kg dry weight. For example:
[GRAPHIC] [TIFF OMITTED] TR18MY12.011

    c. i. Convert from mg of carbon to mg of base fluid. This 
calculation will depend on the % fraction of carbon present in the 
molecular structure of each base fluid. For the control fluids, 
ethyl oleate is composed of 77.3% carbon, hexadecene is composed of 
85.7% carbon, and squalane is composed of 85.3% carbon. The carbon 
fraction of each base fluid should be supplied by the manufacturer 
or determined before use. ASTM D5291-96 or equivalent will be used 
to determine composition of fluid.
    ii. To calculate the amount of base fluid to add to the 
sediment, divide the amount of carbon (480 mg) by the percent 
fraction of carbon in the fluid.
    iii. For example, the amount of ethyl oleate added to 240 g dry 
weight sediment can be calculated from the following equation:

[[Page 29839]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.012

    iv. Therefore, add 621 mg of ethyl oleate to 240 g dry weight 
sediment for a final concentration of 2,000 mg carbon/kg sediment 
dry weight.
    3.1.4. Mix the calculated amount of base fluid with the 
appropriate weight of wet sediment.
    a. Use the wet:dry ratio to convert from g sediment dry weight 
to g sediment wet weight, as follows:
[GRAPHIC] [TIFF OMITTED] TR18MY12.013

    b. i. Weigh the appropriate amount of base fluid (calculated in 
Section 3.1.3.c) into stainless mixing bowls, tare the vessel 
weight, then add the wet sediment calculated in Equation 5, and mix 
with a high shear dispersing impeller for 9 minutes.
    ii. The sediment is now mixed with synthetic sea water to form a 
slurry that will be transferred into the bottles.
    3.2. Creating Seawater/Sediment Slurry
    Given that the total volume of sediment/sea water slurry in each 
bottle is to be 75 mL, determine the volume of sea water to add to 
the wet sediment.
    3.2.1. If each bottle is to contain 30 g dry sediment, calculate 
the weight, and then the volume, of wet sediment to be added to each 
bottle.
[GRAPHIC] [TIFF OMITTED] TR18MY12.014

    3.2.4. Convert the wet sediment weight from Equation 6 into a 
volume using the sediment density.
[GRAPHIC] [TIFF OMITTED] TR18MY12.016

    3.2.5. Determine the amount of sea water to mix with the wet 
sediment.
[GRAPHIC] [TIFF OMITTED] TR18MY12.017

    Mix sea water thoroughly with wet sediment to form a sediment/
sea water slurry.
    3.3. Bottling the Sediment Seawater Slurry
    The total volume of sediment/sea water slurry in each bottle is 
to be 75 mL. Convert the volume (mL) of sediment/sea water slurry 
into a weight (g) using the density of the sediment and the 
seawater.

[[Page 29840]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.018

    This should provide each bottle with 30 g dry sediment in a 
total volume of 75 mL.
    3.3.4. Putting the sediment:seawater slurry in the serum 
bottles.
    a. Note: The slurry will need to be constantly stirred to keep 
the sediment suspended.
    b. Place a tared serum bottle on a balance and add the 
appropriate amount of slurry to the bottle using a funnel. Once the 
required slurry is in the bottle remove the funnel, add 2-3 drops 
(25 [mu]L) of a 1 gram/L resazurin dye stock solution. Cap the 
bottle with a butyl rubber stopper (Bellco Glass, Part 
2048-11800) and crimp with an aluminum seal (Bellco Glass 
Part 2048-11020).
    c. Using a plastic tube with a (23-gauge, 1-inch long) needle 
attached to one side and a nitrogen source to the other, puncture 
the serum cap with the needle. Puncture the serum cap again with a 
second needle to sparge the bottle's headspace of residual air for 
two minutes. The nitrogen should be flowing at no more than 100 mL/
min to encourage gentle displacement of oxygenated air with 
nitrogen. Faster nitrogen flow rates would cause mixing and complete 
oxygen removal would take much longer. Remove the nitrogen needle 
first to avoid any initial pressure problems. The second (vent) 
needle should be removed within 30 seconds of removing the nitrogen 
needle.
    d. Triplicate blank test systems are prepared, with similar 
quantities of sediment and seawater without any base fluid. Incubate 
in the dark at a constant temperature of 29  1 [deg]C.
    e. Record the test temperature. The test duration is dependent 
on base fluid performance, but at a maximum should be no more than 
275 days. Stop the test after all base fluids have achieved a 
plateau of gas production. At termination, base fluid concentrations 
can be verified in the terminated samples by extraction and GC 
analysis according to Section 8.

4.0. Concentration Verification Chemical Analyses

    a. Because of the difficulty of homogeneously mixing base fluid 
with sediment, it is important to demonstrate that the base fluid is 
evenly mixed within the sediment sea water slurry that was added to 
each bottle. Of the seven serum bottles set up for each test or 
control condition, three are randomly selected for concentration 
verification analyses. These should be immediately placed at 4 
[deg]C and a sample of sediment from each bottle should be analyzed 
for base fluid content as soon as possible. The coefficient of 
variation (CV) for the replicate samples must be less than 20%. The 
results should show recovery of at least 70% of the spiked base 
fluid. Use an appropriate analytical procedure described in Section 
8 to perform the extractions and analyses. If any set of sediments 
fail the criteria for concentration verification, then the 
corrective action for that set of sediments is also outlined in 
Section 8.
    b. The nominal concentrations and the measured concentrations 
from the three bottles selected for concentration verification 
should be reported for the initial test concentrations. The 
coefficient of variation (CV) for the replicate samples must be less 
than 20%. If base fluid content results are not within the 20% CV 
limit, the test must be stopped and restarted with adequately mixed 
sediment.

5.0. Gas Monitoring Procedures

    Biodegradation is measured by total gas as specified in ISO 
11734:1995. Methane production can also be tracked and is described 
in Section 7.

5.1. Total Gas Monitoring Procedures

    Bottles should be brought to room temperature before readings 
are taken. a. The bottles are observed to confirm that the resazurin 
has not oxidized to pink or blue. Total gas production in the 
culture bottles should be measured using a pressure transducer (one 
source is Biotech International). The pressure readings from test 
and control cultures are evaluated against a calibration curve 
created by analyzing the pressure created by known additions of gas 
to bottles established identically to the culture bottles. Bottles 
used for the standard curve contain 75 mL of water, and are sealed 
with the same rubber septa and crimp cap seals used for the bottles 
containing sediment. After the bottles used in the standard curve 
have been sealed, a syringe needle inserted through the septa is 
used to equilibrate the pressure inside the bottles to the outside 
atmosphere. The syringe needle is removed and known volumes of air 
are injected into the headspace of the bottles. Pressure readings 
provide a standard curve relating the volume of gas injected into 
the bottles and headspace pressure. No less than three points may be 
used to generate the standard curve. A typical standard curve may 
use 0, 1, 5, 10, 20 and 40 mL of gas added to the standard curve 
bottles.
    b. The room temperature and barometric pressure (to two digits) 
should be recorded at the time of sampling. One option for the 
barometer is Fisher Part 02-400 or 02-401. Gas production 
by the sediment is expressed in terms of the volume (mL) of gas at 
standard temperature (0 [deg]C = 273 [deg]K) and pressure (1 atm = 
30 inches of Hg) using Eq. 16.
[GRAPHIC] [TIFF OMITTED] TR18MY12.020

Where:

V2 = Volume of gas production at standard temperature and 
pressure
P1 = Barometric pressure on day of sampling (inches of 
Hg)
V1 = Volume of gas measured on day of sampling (mL)
T2 = Standard temperature = 273 [deg]K
T1 = Temperature on day of sampling ([deg]C + 273 = 
[deg]K)
P2 = Standard pressure = 30 inches Hg

    c. An estimate can be made of the total volume of anaerobic gas 
that will be produced in the bottles. The gas production measured 
for each base fluid can be expressed as a percent of predicted total 
anaerobic gas production.
    5.1.1. Calculate the total amount of carbon in the form of the 
base fluid present in each bottle.
    a. Each bottle is to contain 30 g dry weight sediment. The base 
fluid concentration is 2,000 mg carbon/kg dry weight sediment. 
Therefore:

[[Page 29841]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.021

    5.1.2. Theory states that anaerobic microorganisms will convert 
1 mole of carbon substrate into 1 mole of total anaerobic gas 
production.
    a. Calculate the number of moles of carbon in each bottle.
    b. The molecular weight of carbon is 12 (i.e., 1 mole of carbon 
= 12 g). Therefore, the number of moles of carbon in each bottle can 
be calculated.
[GRAPHIC] [TIFF OMITTED] TR18MY12.022

    5.1.3. Calculate the predicted volume of anaerobic gas.
    One mole of gas equals 22.4 L (at standard temperature and 
pressure), therefore,
[GRAPHIC] [TIFF OMITTED] TR18MY12.023

5.2. Gas Venting

    a. If the pressure in the serum bottle is too great for the 
pressure transducer or syringe, some of the excess gas must be 
wasted. The best method to do this is to vent the excess gas right 
after measurement. To do this, remove the barrel from a 10-mL 
syringe and fill it \1/3\ full with water. This is then inserted 
into the bottle through the stopper using a small diameter (high 
gauge) needle. The excess pressure is allowed to vent through the 
water until the bubbles stop. This allows equalization of the 
pressure inside the bottle to atmospheric without introducing 
oxygen. The amount of gas vented (which is equal to the volume 
determined that day) must be kept track of each time the bottles are 
vented. A simple way to do this in a spreadsheet format is to have a 
separate column in which cumulative vented gas is tabulated. Each 
time the volume of gas in the cultures is analyzed, the total gas 
produced is equal to the gas in the culture at that time plus the 
total of the vented gas.
    b. To keep track of the methane lost in the venting procedure, 
multiply the amount of gas vented each time by the corrected % 
methane determined on that day. The answer gives the volume of 
methane wasted. This must be added into the cumulative totals 
similarly to the total gas additions.

6.0. Test Acceptability and Interpretation

6.1. Test Acceptability

    At day 275 or when gas production has plateaued, whichever is 
first, the controls are evaluated to confirm that the test has been 
performed appropriately. In order for this modification of the 
closed bottle biodegradation test to be considered acceptable, all 
the controls must meet the biodegradation levels indicated in Table 
1. The intermediate control hexadecene must produce at least 30% of 
the theoretical gas production. This level may be reexamined after 
two years and more data has been generated.

                                      Table 1--Test Acceptability Criteria
----------------------------------------------------------------------------------------------------------------
           Concentration                      Percent biodegradability as a function of gas measurement
----------------------------------------------------------------------------------------------------------------
                                                                Squalane negative      Hexadecene intermediate
                                        Positive control             control                   control
----------------------------------------------------------------------------------------------------------------
2,000 mg carbon/kg.................  >=60% theoretical.....  <=5% theoretical......  >=30% theoretical.
----------------------------------------------------------------------------------------------------------------

6.2 Interpretation

    a. In order for a fluid to pass the closed bottle test, the 
biodegradation of the base fluid as indicated by the total amount of 
total gas (or methane) generated once gas production has plateaued 
(or at the end of 275 days, which ever is first) must be greater 
than or equal to the volume of gas (or methane) produced by the 
reference standard (internal elefin or ester).
    b. The method for evaluating the data to determine whether a 
fluid has passed the biodegradation test must use the equations:
[GRAPHIC] [TIFF OMITTED] TR18MY12.024

Where:

NAF = Stock base fluid being tested for compliance
Reference fluid = C16-C18 internal olefin or 
C12 -C14 or C8 ester reference 
fluid

7.0. Methane Measurement

7.1. Methane Monitoring Procedures

    a. The use of total gas production alone may result in an 
underestimation of the actual metabolism occurring since 
CO2 is slightly soluble in water. An acceptable 
alternative method is to monitor methane production and total gas 
production. This is easily done using GC analysis. A direct 
injection of headspace gases can be made into a GC using almost any 
packed or capillary column with an FID detector. Unless volatile 
fuels or solvents are present in the test material or the inocula, 
the only component of the headspace gas that can be detected using 
an FID detector is methane. The percent methane in the headspace gas 
is determined by comparing the response of the sample injections to 
the response from injections of known percent methane standards. The 
percent methane is corrected for water vapor saturation using Eq. 21 
and then converted to a volume of dry methane using Eq. 22.

[[Page 29842]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.025

Where:

D = The density of water vapor at saturation (g/m\3\, can be found 
in CRC Handbook of Chemistry and Physics) for the temperature of 
sampling.
[GRAPHIC] [TIFF OMITTED] TR18MY12.026

Where:

VCH4 = Volume of methane in the bottle
S = Volume of excess gas production (measured with a pressure 
transducer)
V = Volume of the headspace in the culture bottle (total volume--
liquid phase)
P = Barometric pressure (mm Hg, measured with barometer)
T = Temperature ([deg]C)
Pw = Vapor pressure of water at T (mm Hg, can be found in 
CRC Handbook of Chemistry and Physics)
CH4 = % methane in headspace gas (after correction for 
water vapor)

    b. The total volume of serum bottles sold as 125 mL bottles 
(Wheaton) is 154.8 mL.
    c. The volumes of methane produced are then compared to the 
volumes of methane in the controls to determine if a significant 
inhibition of methane production or a significant increase of 
methane production has been observed. Effective statistical analyses 
are important, as variability in the results is common due to the 
heterogeneity of the inoculum's source. It is also common to observe 
that the timing of the initiation of culture activity is not equal 
in all of the cultures. Expect a great variability over the period 
when the cultures are active, some replicates will start sooner than 
others, but all of the replicates should eventually reach similar 
levels of base fluid degradation and methane production.

7.2. Expected Methane Production Calculations

    a. The amount of methane expected can be calculated using the 
equation of Symons and Buswell (Eq. 23). In the case of complete 
mineralization, all of the carbon will appear as wither 
CO2 or CH4, thus the total moles of gas 
produced will be equal to the total moles of carbon in the parent 
molecule. The use of the Buswell equation allows you to calculate 
the effects the redox potential will have on the distribution of the 
products in methanogenic cultures. More reduced electron donors will 
allow the production of more methane, while more oxidized electron 
donors will cause a production of more carbon dioxide.
[GRAPHIC] [TIFF OMITTED] TR18MY12.027

    b. An example calculation of the expected methane volume in a 
culture fed 2,000 mg/kg hexadecene is as follows. The application of 
Symons and Buswell's equation reveals that hexadecene 
(C16H32) will yield 4 moles of CO2 
and 12 moles of CH4. Assuming 30 g of dry sediment are 
added to the bottles with 2,334 mg hexadecene/kg dry sediment (i.e., 
equivalent to 2,000 mg carbon/kg dry sediment) the calculation is as 
follows.
[GRAPHIC] [TIFF OMITTED] TR18MY12.028

    c. By subtracting the average amount of methane in control 
bottles from the test bottles and then dividing by the expected 
volume an evaluation of the completion of the process may be 
conducted.

8.0. Concentration Verification Analysis

    The Concentration Verification analysis is required at the 
beginning of the test to ensure homogeneity and confirm that the 
required amount of fluid was delivered to the sediments at the start 
of the test.
    8.1. Three samples per fluid need to be analyzed and achieve 
<=20% Coefficient of Variability and an average of >=70% to <=120% 
of fluid delivered to sediment.
    8.2. If a third party performs the analysis, then the laboratory 
should be capable of delivering the homogeneity data within seven 
days, in order to identify any samples that do not meet the 
homogeneity requirement as quickly as possible.
    8.3. If one sediment/fluid set, out a multiple set batch of 
samples, fails these criteria, then that one set of samples must be 
discarded and a fresh set of spiked sediment prepared, started, and 
analyzed to ensure homogeneity. The same stock sediment is used to 
prepare the replacement set(s). The remaining sets do not need to be 
re-mixed or restarted.
    8.4. The re-mixed set(s) will need to be run the additional days 
as appropriate to ensure that the total number of days is the same 
for all sets of bottles, even though the specific days are not 
aligned.
    8.5. Re-mixing of bottle sets can be performed multiple times as 
a result of a failure of the analytical criteria, until the holding 
time for the stock sediment has expired (60 days). If the problem 
set(s) has not fallen within the acceptable analytical criteria by 
then, it must not be part of the batch of bottles run. If the 
problem batch is one of the controls, and those controls were not 
successfully prepared when the sediment holding time expired, then 
the entire test must be restarted.

9.0 Program Quality Assurance and Quality Control

9.1 Calibration

    9.1.1. All equipment/instrumentation will be calibrated in 
accordance with the test method or the manufacturer's instructions 
and may be scheduled or triggered.
    9.1.2. Where possible, standards used in calibration will be 
traceable to a nationally recognized standard (e.g., certified 
standard by NIST).
    9.1.3. All calibration activities will be documented and the 
records retained.
    9.1.4. The source, lot, batch number, and expiration date of all 
reagents used with be documented and retained.

[[Page 29843]]

9.2. Maintenance

    9.2.1. All equipment/instrumentation will be maintained in 
accordance with the test method or the manufacturer's instructions 
and may be scheduled or triggered.
    9.2.2. All maintenance activities will be documented and the 
records retained.

9.3. Data Management and Handling

    9.3.1. All primary (raw) data will be correct, complete, without 
selective reporting, and will be maintained.
    9.3.2. Hand-written data will be recorded in lab notebooks or 
electronically at the time of observation.
    9.3.3. All hand-written records will be legible and amenable to 
reproduction by electrostatic copiers.
    9.3.4. All changes to data or other records will be made by:
    a. Using a single line to mark-through the erroneous entry 
(maintaining original data legibility).
    b. Write the revision.
    c. Initial, date, and provide revision code (see attached or 
laboratory's equivalent).
    9.3.5. All data entry, transcriptions, and calculations will be 
verified by a qualified person.
    a. Verification will be documented by initials of verifier and 
date.
    9.3.6. Procedures will be in place to address data management 
procedures used (at minimum):
    a. Significant figures.
    b. Rounding practices.
    c. Identification of outliers in data series.
    d. Required statistics.

9.4. Document Control

    9.4.1. All technical procedures, methods, work instructions, 
standard operating procedures must be documented and approved by 
laboratory management prior to the implementation.
    9.4.2. All primary data will be maintained by the contractor for 
a minimum of five (5) years.

9.5. Personnel and Training

    9.5.1. Only qualified personnel shall perform laboratory 
activities.
    9.5.2. Records of staff training and experience will be 
available. This will include initial and refresher training (as 
appropriate).

9.6. Test Performance

    9.6.1. All testing will done in accordance with the specified 
test methods.
    9.6.2. Receipt, arrival condition, storage conditions, 
dispersal, and accountability of the test article will be documented 
and maintained.
    9.6.3. Receipt or production, arrival or initial condition, 
storage conditions, dispersal, and accountability of the test matrix 
(e.g., sediment or artificial seawater) will be documented and 
maintained.
    9.6.4. Source, receipt, arrival condition, storage conditions, 
dispersal, and accountability of the test organisms (including 
inoculum) will be documented and maintained.
    9.6.5. Actual concentrations administered at each treatment 
level will be verified by appropriate methodologies.
    9.6.6. Any data originating at a different laboratory will be 
identified and the laboratory fully referenced in the final report.

9.7. The following references identify analytical methods that have 
historically been successful for achieving the analytical quality 
criteria.

    9.7.1. Continental Shelf Associates Report 1998. Joint EPA/
Industry Screening Survey to Assess the Deposition of Drill Cuttings 
and Associated Synthetic Based Mud on the Seabed of the Louisiana 
Continental Shelf, Gulf of Mexico. Analysis by Charlie Henry Report 
Number IES/RCAT97-36 GC-FID and GC/MS.
    9.7.2. EPA Method 3550 for extraction with EPA Method 8015 for 
GC-FID. EPA Method 3550C, Revision 3. February 2007. Ultrasonic 
Extraction. EPA Method 8015C, Revision 3. February 2007. 
Nonhalogenated Organics by Gas Chromatography.
    9.7.3. Chandler, J.E., S.P. Rabke, and A.J.J. Leuterman. 1999. 
Predicting the Potential Impact of Synthetic-Based Muds With the Use 
of Biodegradation Studies. Society of Petroleum Engineers SPE 52742.
    9.7.4. Chandler, J.E., B. Lee, S.P. Rabke, J.M. Geliff, R. 
Stauffer, and J. Hein. 2000. Modification of a Standardized 
Anaerobic Biodegradation Test to Discriminate Performance of Various 
Non-Aqueous Base Fluids. Society of Petroleum Engineers SPE 61203.
    9.7.5. Munro, P.D., B Croce, C.F. Moffet, N.A Brown, A.D. 
McIntosh, S.J. Hird, and R.M. Stagg. 1998. Solid-Phase Test for 
Comparison for Degradation Rates of Synthetic Mud Base Fluids Used 
in the Off-shore Drilling Industry. Environ. Toxicol. Chem. 17:1951-
1959.
    9.7.6. Webster, L., P.R. Mackie, S.J. Hird, P.D. Munro, N.A. 
Brown, and C.F. Moffat. 1997. Development of Analytical Methods for 
the Determination of Synthetic Mud Base Fluids in Marine Sediments. 
The Analyst 122:1485-1490.
    9.8 The following standards are approved for incorporation by 
reference by the Director of the Federal Register in accordance with 
5 U.S.C. 552(a) and 1 CFR part 51. Copies may also be inspected at 
EPA's Water Docket, 1200 Pennsylvania Ave. NW., Washington, DC 20460 
and at at the National Archives and Records Administration (NARA). 
For information on the availability of this material at NARA, call 
202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
    9.8.1 ASTM International. Available from ASTM International, 100 
Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, 
or online at http://www.astm.org.
    9.8.1.1 ASTM D5291-96, Standard Test Methods for Instrumental 
Determination of Carbon, Hydrogen, and Nitrogen in Petroleum 
Products and Lubricants, approved April 10, 1996.
    9.8.1.2 ASTM D2974-07a, Standard Test Methods for Moisture, Ash, 
and Organic Matter of Peat and Other Organic Soils, approved March 
15, 2007.

0
26. Amend Appendix 5 to Subpart A of Part 435 by:
0
a. Revising the appendix heading.
0
b. Removing ``35 to 500 amu'' and adding in its place ``35 to 600 amu'' 
in Section 6.3.2.
0
c. Revising section 9.5. introductory text.
0
d. Revising the equation in section 9.5.2.
0
e. Revising sections 9.6, 11.3 introductory text, 11.3.1, and 11.5.4.2.
0
f. Adding section 6.17.

Appendix 5 to Subpart A of Part 435-- Determination of Crude Oil 
Contamination in Non-Aqueous Drilling Fluids by Gas Chromatography/Mass 
Spectrometry (GC/MS) (EPA Method 1655)

* * * * *
    9.5 Duplicates--A duplicate field sample shall be prepared and 
analyzed according to Section 11. The relative percent difference 
(RPD) of the calculated concentrations shall be less than 15%.
* * * * *
[GRAPHIC] [TIFF OMITTED] TR18MY12.029

    9.6 A clean NAF sample shall be prepared and analyzed according 
to Section 11. Ultimately the oil-equivalent concentration from the 
TIC or EIP signal measured in the clean NAF sample shall be 
subtracted from the corresponding authentic field samples in order 
to calculate the true contaminant concentration (% oil) in the field 
samples (see Section 12).
* * * * *
    11.3 Qualitative Identification--See Section 17 of this method 
for schematic flowchart.
    11.3.1 Qualitative identification shall be accomplished by 
comparison of the TIC and EIP area data from an authentic sample to 
the TIC and EIP area data from the calibration standards (see 
Section 10.4). Crude oil shall be identified by the presence of 
C10 to C13 n-alkanes and corresponding target 
aromatics.
* * * * *
    11.5.4.2 Asphaltene crude oils with API gravity <20 may not 
produce chromatographic peaks strong enough to show contamination at 
levels of the calibration. Extracted ion peaks should be easier to 
see than increased intensities for the C8 to C13 peaks. If a sample 
of asphaltene crude from the formation is available, a calibration 
standard shall be prepared.
BILLING CODE 6560-50-P

[[Page 29844]]

[GRAPHIC] [TIFF OMITTED] TR18MY12.030


[[Page 29845]]


BILLING CODE 6560-50-C

0
27. The heading of Appendix 6 to Subpart A of Part 435 is revised to 
read as follows:

Appendix 6 to Subpart A of Part 435-- Reverse Phase Extraction (RPE) 
Method for Detection of Oil Contamination in Non-Aqueous Drilling 
Fluids (NAF) (GC/MS) (EPA Method 1670)

* * * * *

0
28. The heading of Appendix 7 to Subpart A of Part 435 is revised to 
read as follows:

Appendix 7 to Subpart A of Part 435-- Determination of the Amount of 
Non-Aqueous Drilling Fluid (NAF) Base Fluid From Drill Cuttings by a 
Retort Chamber (Derived From API Recommended Practice 13B-2) (EPA 
Method 1674)

* * * * *

0
29. Appendix 8 to Subpart A of Part 435 is amended by:
0
a. Revising the second paragraph.
0
b. Adding ``>'' before ``11-14'' in Table 1.

Appendix 8 to Subpart A of Part 435--Reference C16-
C18 Internal Olefin Drilling Fluid Formulation

* * * * *
    Drilling fluid sediment toxicity ratio = 4-day LC50 
of C16-C18 internal olefin drilling fluid/4-
day LC50 of drilling fluid removed from drill cuttings at 
the solids control equipment as determined by EPA Method 1644: 
``Method for Conducting a Sediment Toxicity Test with Leptocheirus 
plumulosus and Non-Aqueous Drilling Fluids or Synthetic-Based 
Drilling Muds'' after sediment preparation procedures specified in 
EPA Method 1646, which are published as appendices to Subpart A of 
this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See Sec.  435.11(ee) and 
(uu).
* * * * *

Subpart D--Coastal Subcategory

0
30. Section 435.41 is amended:
0
a. By revising paragraph (d).
0
b. By revising paragraph (e).
0
c. By revising paragraph (k).
0
d. By revising paragraph (m)(2).
0
e. By revising paragraph (q).
0
f. By revising paragraph (r).
0
g. By amending paragraph (w) to remove ``LC5'' and add in 
its place ``LC50''.
0
h. By revising paragraph (y).
0
i. By revising paragraph (ee).
0
j. By revising paragraph (ff).
0
k. By adding paragraph (mm).


Sec.  435.41  Special definitions.

* * * * *
    (d) Base fluid retained on cuttings as applied to BAT effluent 
limitations and NSPS refers to the ``Determination of the Amount of 
Non-Aqueous Drilling Fluid (NAF) Base Fluid from Drill Cuttings by a 
Retort Chamber (Derived from API Recommended Practice 13B-2)'', EPA 
Method 1674, which is published as an appendix to Subpart A of this 
part and in ``Analytic Methods for the Oil and Gas Extraction Point 
Source Category,'' EPA-821-R-11-004. See paragraph (mm) of this 
section.
    (e) Biodegradation rate as applied to BAT effluent limitations and 
NSPS for drilling fluids and drill cuttings refers to the ``Protocol 
for the Determination of Degradation of Non Aqueous Base Fluids in a 
Marine Closed Bottle Biodegradation Test System: Modified ISO 
11734:1995,'' EPA Method 1647, supplemented with ``Procedure for Mixing 
Base Fluids With Sediments,'' EPA Method 1646. Both EPA Method 1646 and 
1647 are published as appendices to Subpart A of this part and in 
``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See paragraph (mm) of this section.
* * * * *
    (k) Diesel oil refers to the grade of distillate fuel oil, as 
specified in the American Society for Testing and Materials Standard 
Specification for Diesel Fuel Oils D975-91, that is typically used as 
the continuous phase in conventional oil-based drilling fluids. This 
incorporation by reference was approved by the Director of the Federal 
Register in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies 
may be obtained from the American Society for Testing and Materials, 
100 Barr Harbor Drive, West Conshohocken, PA 19428. Copies may be 
inspected at the National Archives and Records Administration (NARA). 
For information on the availability of this material at NARA, call 202-
741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be 
inspected at EPA's Water Docket, 1200 Pennsylvania Ave. NW., 
Washington, DC 20460.
* * * * *
    (m) * * *
    (2) Dry drill cuttings means the residue remaining in the retort 
vessel after completing the retort procedure specified in EPA Method 
1674, which is published as an appendix to Subpart A of this part and 
in ``Analytic Methods for the Oil and Gas Extraction Point Source 
Category,'' EPA-821-R-11-004. See paragraph (mm) of this section.
* * * * *
    (q) Formation oil means the oil from a producing formation which is 
detected in the drilling fluid, as determined by the GC/MS compliance 
assurance method, EPA Method 1655, when the drilling fluid is analyzed 
before being shipped offshore, and as determined by the RPE method, EPA 
Method 1670, when the drilling fluid is analyzed at the offshore point 
of discharge. The GC/MS compliance assurance method and the RPE method 
approved for use with this part are published as appendices to Subpart 
A of this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See paragraph (mm) of this 
section. Detection of formation oil by the RPE method may be confirmed 
by the GC/MS compliance assurance method, and the results of the GC/MS 
compliance assurance method shall supersede those of the RPE method.
    (r) Garbage means all kinds of victual, domestic, and operational 
waste, excluding fresh fish and parts thereof, generated during the 
normal operation of coastal oil and gas facility and liable to be 
disposed of continuously or periodically, except dishwater, graywater, 
and those substances that are defined or listed in other Annexes to 
MARPOL 73/78. A copy of MARPOL may be inspected at EPA's Water Docket, 
1200 Pennsylvania Ave. NW., Washington, DC 20460.
* * * * *
    (y) No discharge of free oil means that waste streams may not be 
discharged that contain free oil as evidenced by the monitoring method 
specified for that particular stream, e.g., deck drainage or 
miscellaneous discharges cannot be discharged when they would cause a 
film or sheen upon or discoloration of the surface of the receiving 
water; drilling fluids or cuttings may not be discharged when they fail 
EPA Method 1617 (Static Sheen Test), which is published as an appendix 
to Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph 
(mm) of this section.
* * * * *
    (ee) SPP toxicity as applied to BAT effluent limitations and NSPS 
for drilling fluids and drill cuttings refers to the bioassay test 
procedure, ``Suspended Particulate Phase (SPP) Toxicity Test,'' 
presented in EPA Method 1619, which is published as an appendix to 
Subpart A of this part and in ``Analytic Methods for the Oil and Gas 
Extraction Point Source Category,'' EPA-821-R-11-004. See paragraph 
(mm) of this section.
    (ff) Static sheen test means the standard test procedure that has 
been

[[Page 29846]]

developed for this industrial subcategory for the purpose of 
demonstrating compliance with the requirement of no discharge of free 
oil. The methodology for performing the static sheen test is presented 
in EPA Method 1617, which is published as an appendix to Subpart A of 
this part and in ``Analytic Methods for the Oil and Gas Extraction 
Point Source Category,'' EPA-821-R-11-004. See paragraph (mm) of this 
section.
* * * * *
    (mm) Analytic Methods for the Oil and Gas Extraction Point Source 
Category is the EPA document, EPA-821-R-11-004, that compiles analytic 
methods for this category. Copies may be inspected at the National 
Archives and Records Administration (NARA). For information on the 
availability of this material at NARA, call 202-741-6030, or go to: 
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. A copy may also be inspected at EPA's 
Water Docket, 1200 Pennsylvania Ave. NW., Washington, DC 20460. This 
method may be obtained at http://water.epa.gov/scitech/methods/cwa/index.cfm.

0
31. In Sec.  435.42 footnote 1 to the table is revised to read as 
follows:


Sec.  435.42  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
practicable control technology currently available (BPT).

* * * * *
    \1\ No discharge of free oil. See Sec.  435.41(y).
* * * * *

0
32. In Sec.  435.43:
0
a. Remove ``LC5'' and add in its place ``LC50'' 
in the table.
0
b. Footnotes 2 and 4 to the table are revised to read as follows:


Sec.  435.43  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
available technology economically achievable (BAT).

* * * * *
    \2\ As determined by the static sheen test. See Sec.  
435.41(ff).
* * * * *
    \4\ As determined by the suspended particulate phase (SPP) 
toxicity test. See Sec.  435.41(ee).
* * * * *

0
33. In Sec.  435.44 footnote 2 to the table is revised to read as 
follows:


Sec.  435.44  Effluent limitations guidelines representing the degree 
of effluent reduction attainable by the application of the best 
conventional pollutant control technology (BCT).

* * * * *
    \2\ As determined by the static sheen test. See Sec.  
435.41(ff).
* * * * *

0
34. In Sec.  435.45:
0
a. Remove ``LC5'' and add in its place ``LC50''in 
the table.
0
b. Footnotes 2 and 4 to the table are revised to read as follows:


Sec.  435.45  Standards of performance for new sources (NSPS).

* * * * *
    \2\ As determined by the static sheen test. See Sec.  
435.41(ff).
* * * * *
    \4\ As determined by the suspended particulate phase (SPP) 
toxicity test. See Sec.  435.41(ee).
* * * * *
[FR Doc. 2012-10210 Filed 5-17-12; 8:45 am]
BILLING CODE 6560-50-P