Thursday, 

September 23, 2010 

Part II 

Environmental 

Protection Agency 

40 CFR Parts 136, 260, 423, et al. 

Guidelines Establishing Test Procedures 

for the Analysis of Pollutants Under the 

Clean Water Act; Analysis and Sampling 

Procedures; Proposed Rule 

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58024 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

ENVIRONMENTAL PROTECTION 

AGENCY 

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

435 

[EPA–HQ–OW–2010–0192; FRL–9189–4] 

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: Proposed rule. 

SUMMARY: EPA is proposing changes to 

analysis and sampling test procedures 

in wastewater regulations. These 

changes will provide increased 

flexibility to the regulated community 

and laboratories in their selection of 

analytical methods (test procedures) for 

use in Clean Water Act programs. The 

changes include proposal of EPA 

methods and methods published by 

voluntary consensus standard bodies, 

such as ASTM International and the 

Standard Methods Committee and 

updated versions of currently approved 

methods. EPA is also proposing to add 

certain methods reviewed under the 

alternate test procedures program. 

Further, EPA is proposing changes to 

the current regulations to clarify the 

process for EPA approval for use of 

alternate procedures for nationwide and 

Regional use. In addition, EPA is 

proposing minimum quality control 

requirements to improve consistency 

across method versions; corrections to 

previously approved methods; and 

changes to sample collection, 

preservation, and holding time 

requirements. Finally, EPA is proposing 

changes to how EPA cites methods in 

three effluent guideline regulations. 

DATES: EPA must receive your 

comments on this proposal on or before 

November 22, 2010. 

ADDRESSES: Submit your comments, 

identified by Docket ID No. EPA–HQ– 

OW–2010–0192, by one of the following 

methods: 

• http://www.regulations.gov: Follow 

the on-line instructions for submitting 

comments. 

• E-mail: OW-Docket@epa.gov, 

Attention Docket ID No. EPA–HQ–OW– 

2010–0192. 

• Mail: Water Docket, U.S. 

Environmental Protection Agency, 

Mailcode: 2822T, 1200 Pennsylvania 

Ave., NW., Washington, DC 20460. 

Attention Docket ID No. EPA–HQ–OW– 

2010–0192. Please include a total of 

3 copies. 

• Hand Delivery: Water Docket, EPA 

Docket Center, EPA West Building 

Room 3334, 1301 Constitution Ave., 

NW., Washington, DC, Attention Docket 

ID No. EPA–HQ–OW–2010–0192. Such 

deliveries are only accepted during the 

Docket’s normal hours of operation, and 

special arrangements should be made 

for deliveries of boxed information by 

calling 202–566–2426. 

Instructions: Direct your comments to 

Docket ID No. EPA–HQ–OW–2010– 

0192. EPA’s policy is that all comments 

received will be included in the public 

docket without change and may be 

made available online at http:// 

www.regulations.gov, including any 

personal information provided, unless 

the comment includes information 

claimed to be Confidential Business 

Information (CBI) or other information 

whose disclosure is restricted by statute. 

Do not submit information that you 

consider to be CBI or otherwise 

protected through http:// 

www.regulations.gov or e-mail. The 

http://www.regulations.gov Web site is 

an ‘‘anonymous access’’ system, which 

means EPA will not know your identity 

or contact information unless you 

provide it in the body of your comment. 

If you send an e-mail comment directly 

to EPA without going through http:// 

www.regulations.gov your e-mail 

address will be automatically captured 

and included as part of the comment 

that is placed in the public docket and 

made available on the Internet. If you 

submit an electronic comment, EPA 

recommends that you include your 

name and other contact information in 

the body of your comment and with any 

disk or CD–ROM you submit. If EPA 

cannot read your comment due to 

technical difficulties and cannot contact 

you for clarification, EPA may not be 

able to consider your comment. 

Electronic files should avoid the use of 

special characters, any form of 

encryption, and be free of any defects or 

viruses. 

Docket: All documents in the docket 

are listed in the http:// 

www.regulations.gov index. Although 

listed in the index, some information is 

not publicly available, e.g., CBI or other 

information whose disclosure is 

restricted by statute. Certain other 

material, such as copyrighted material, 

will be publicly available only in hard 

copy. Publicly available docket 

materials are available either 

electronically in http:// 

www.regulations.gov or in hard copy at 

the Water Docket in the EPA 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 for 

the Water Docket is 202–566–2426. 

FOR FURTHER INFORMATION CONTACT: 

Lemuel Walker, Engineering and 

Analysis Division (4303T), USEPA 

Office of Science and Technology, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460, 202–566–1077, (e-mail: 

walker.lemuel@epa.gov), or Meghan 

Hessenauer, Engineering and Analysis 

Division (4303T), USEPA Office of 

Science and Technology, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460, 202–566–1040 (e-mail: 

hessenauer.meghan@epa.gov). 

SUPPLEMENTARY INFORMATION: 

A. General Information 

1. Does this action apply to me? 

This proposed rule could affect a 

number of different entities. Potential 

regulators may include EPA Regions, as 

well as States, Territories and Tribes 

authorized to implement the National 

Pollutant Discharge Elimination System 

(NPDES) program, and 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 permitee must use 

an approved test procedure (or an 

approved alternate test procedure) 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 regulated by the 

actions in this rulemaking. Categories 

and entities that may potentially be 

subject to the requirements of today’s 

rule include: 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58025 

Category Examples of potentially regulated entities 

State, Territorial, and Indian Tribal Governments ... States, Territories, and Tribes authorized to administer the NPDES permitting program; 

States, Territories, and Tribes providing certification under Clean Water Act section 401. 

Industry ..................................................................... Facilities that must conduct monitoring to comply with NPDES permits. 

Municipalities ............................................................ POTWs 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 

regulated by this action. This table lists 

types of entities that EPA is now aware 

that could potentially be regulated by 

this action. Other types of entities not 

listed in the table could also be 

regulated. To determine whether your 

facility is regulated by this action, you 

should carefully examine the 

applicability language at 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 should I consider as I prepare 

my comments for EPA? 

1. Submitting Confidential Business 

Information (CBI). Do not submit this 

information to EPA through http:// 

www.regulations.gov or e-mail. Clearly 

mark the part or all of the information 

that you claim to be CBI. For CBI 

information in a disk or CD–ROM that 

you mail to EPA, mark the outside of the 

disk or CD–ROM as CBI and then 

identify electronically within the disk or 

CD–ROM the specific information that 

is claimed as CBI. In addition to one 

complete version of the comment that 

includes information claimed as CBI, a 

copy of the comment that does not 

contain the information claimed as CBI 

must be submitted for inclusion in the 

public docket. Information so marked 

will not be disclosed except in 

accordance with procedures set forth in 

40 CFR part 2. 

2. Tips for Preparing Your Comments. 

When submitting comments, remember 

to: 

• Identify the rulemaking by docket 

number and other identifying 

information (subject heading, Federal 

Register date and page number). 

• Follow directions—The agency may 

ask you to respond to specific questions 

or organize comments by referencing a 

Code of Federal Regulations (CFR) part 

or section number. 

• Explain why you agree or disagree, 

suggest alternatives, and substitute 

language for your requested changes. 

• Describe any assumptions and 

provide any technical information and/ 

or data that you used. 

• If you estimate potential costs or 

burdens, explain how you arrived at 

your estimate in sufficient detail to 

allow for it to be reproduced. 

• Provide specific examples to 

illustrate your concerns, and suggest 

alternatives. 

• Explain your views as clearly as 

possible, avoiding the use of profanity 

or personal threats. 

• Make sure to submit your 

comments by the comment period 

deadline identified. 

C. Abbreviations and Acronyms Used 

in the Preamble and Proposed Rule 

Text 

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 PlasmaAtomic Emission Spectroscopy 

ICP/MS: Inductively Coupled Plasma-Mass 

Spectrometry 

MS: Mass Spectrometry 

NPDES: National Pollutant Discharge 

Elimination System 

QA: Quality Assurance 

QC: Quality Control 

SDWA: Safe Drinking Water Act 

SM: Standard Methods 

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 Proposed Rule 

A. Changes to 40 CFR 136.3 To Include 

New EPA Methods and New Versions of 

Previously Approved EPA Methods 

B. Changes to 40 CFR 136.3 To Include 

New Standard Methods and New 

Versions of Approved Standard Methods 

C. Changes to 40 CFR 136.3 To Include 

New ASTM Methods or New Versions of 

Previously Approved ASTM Methods 

D. Changes to 40 CFR 136.3 To Include 

Alternate Test Procedures 

E. Clarifications and Corrections to 

Previously Approved Methods in 40 CFR 

136.3 

F. Proposed Revisions in Table II at 40 CFR 

136.3(e) to Required Containers, 

Preservation Techniques, and Holding 

Times 

G. Proposed Revisions to 40 CFR 136.4 and 

136.5 

H. Proposed Revisions to Method 

Modification Provisions at 40 CFR 136.6 

I. Proposed New Quality Assurance and 

Quality Control Language at 40 CFR 

136.7 

J. Proposed Withdrawal of Appendices at 

40 CFR 136 

K. Proposed Revisions to 40 CFR 423 

L. Proposed Revisions to 40 CFR 430 

M. Proposed Revisions to 40 CFR 435 

III. Statutory and Executive Order Reviews 

A. Executive Order 12866: Regulatory 

Planning and 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 

IV. References 

I. Statutory Authority 

EPA is proposing 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 

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58026 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

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 Proposed Rule 

EPA’s regulations at 40 CFR part 136 

identify test procedures that must be 

used for the analysis of pollutants in all 

applications and report under the CWA 

NPDES program as well as State 

certifications pursuant to section 401 of 

the CWA. Included among the approved 

test procedures are analytical methods 

developed by EPA as well as methods 

developed by voluntary standards 

development organizations such as 

ASTM International and by the joint 

efforts of the Standard Methods 

Committee which is comprised of three 

technical societies (American Public 

Health Association, American Water 

Works Association and the Water 

Environment Federation) and produce 

Standard Methods for the Examination 

of Water and Wastewater. EPA approves 

analytical methods (test procedures) for 

measuring regulated pollutants in 

wastewater. Regulated and regulatory 

entities use these approved methods for 

determining compliance with NPDES 

permits or other monitoring 

requirements. Often, these entities have 

a choice in deciding which approved 

method they will use because EPA has 

approved the use of more than one 

method. This rule proposes to add to 

this list of approved methods. 

Associated with the proposed approved 

methods are their regulated analytes 

(parameters) within the method. Some 

of these proposed methods introduce 

new technologies to the NPDES 

program, while others are updated 

versions of previously approved 

methods. These additions will improve 

data quality and provide the regulated 

community with greater flexibility. 

Further, EPA is aware that organizations 

sometimes republish methods to correct 

errors or revise the description. These 

changes do not affect the performance of 

the method. Therefore, if there are 

changes for methods in this proposed 

rule before publication of a final rule, 

EPA will include the updated versions. 

In the tables at Section 136.3, EPA lists 

the parameters in alphabetical order. To 

better identify new parameters proposed 

in this rule EPA added some of these 

parameters, such as bisphenol A and 

nonylphenol, at the end of these lists. In 

the final rule, EPA may choose to 

reorder the listings to arrange all 

parameters alphabetically. 

A. Changes to 40 CFR 136.3 To Include 

New EPA Methods and New Versions of 

Previously Approved EPA Methods 

EPA is proposing to add new EPA 

methods that require new technologies 

to its Part 136 test procedures. EPA also 

is proposing new versions of already 

approved EPA methods with 

technologies that have been in use for 

many years. The new EPA methods and 

new versions of EPA approved methods 

are described in the following 

paragraphs. 

1. EPA is proposing a new version of 

EPA Method 1664, 1664B: N-Hexane 

Extractable Material (HEM; Oil and 

Grease) and Silica Gel Treated NHexane Extractable Material (SGT– 

HEM; Non-polar Material) by Extraction 

and Gravimetry for use in CWA 

programs. In addition, EPA is proposing 

to amend the RCRA regulations at 40 

CFR 260.11, which currently specify use 

of method 1664A, to additionally 

specify the revised version, 1664B. 

Currently, Method 1664A is used as a 

required testing method to determine 

eligibility of materials for certain 

conditional exclusions from RCRA 

regulations under 40 CFR 260.20 and 

260.22. These exclusions are known as 

‘‘delistings.’’ These delistings provide 

that certain wastes generated at 

particular facilities are no longer 

classified as hazardous wastes under 

RCRA. When delistings are granted by 

EPA, the Agency describes them, along 

with applicable conditions, in appendix 

IX to 40 CFR part 261. 

A number of delistings specify, among 

other things, the following test method: 

‘‘Method 9070A (uses EPA Method 

1664, Rev. A).’’ This testing method 

must be used by waste generators to 

determine if their wastes are an oily 

waste for delisting purposes. The 

language used in Appendix IX reads this 

way because Method 9070A in SW–846 

(including on the SW–846 Web site, 

http://www.epa.gov/epawaste/hazard/

testmethods/sw846/pdfs/9070a.pdf ) 

simply reads that Method 1664A is to be 

used. Thus, although Method 9070A is 

cited, it is actually Method 1664A. 

Method 9070A does not exist 

independently of Method 1664A. 

Once this rule becomes final, we 

would encourage future delistings, if 

applicable, to cite the test method as 

‘‘Method 9070A (uses Method EPA 

1664, Rev. B).’’ EPA is not proposing to 

amend delistings granted in previous 

years that reference Method 1664A at 

this time, since it would require 

additional review to assess the need for 

such a change and an analysis of each 

delisting. 

Oil and Grease is a method-defined 

parameter that measures hexane 

extractable material (HEM) using nhexane (85% minimum purity, 99.0% 

minimum saturated C6 isomer, residue 

< 1mg/L.) Before the use of Freon® was 

banned, EPA defined oil and grease as 

Freon®-extractable material. To replace 

Freon® for oil and grease determinations 

(64 FR 26315, May 14, 1999) EPA 

conducted extensive side-by-side 

studies of several extracting solvents on 

a variety of samples to determine how 

the values compared to Freon®- 

extractable material values. 

In today’s proposed rule, EPA 

describes six oil and grease methods, 

and proposes only the three methods in 

Table IB that use n-hexane to extract the 

sample because the solvent-defined 

definition of oil and grease 

measurements precludes use of any 

other extraction solvent or extraction 

technique. Without extensive side-byside testing, permit writers, permitees, 

and data reviewers lack a basis for 

comparing HEM permit limits or 

measurements to values obtained with 

other extraction solvents or techniques. 

EPA lacks information about whether 

permit writers or permitees would value 

having more ways to extract oil and 

grease samples, or about how much 

effort they or others would be willing to 

exert to determine if the alternate values 

were equal to HEM values or convertible 

to HEM values by a conversion factor. 

Although solvents may not be 

changed, EPA has described some 

allowable changes to the proposed EPA 

Method 1664B. This method describes 

(1) modifications allowable for 

nationwide use without prior EPA 

reviews (cf. documentation procedures 

described at 40 CFR 136.6), and (2) 

describes modifications not allowable 

including the use of any extraction 

solvent other than n-hexane or 

determination technique other than 

gravimetry. Although Method 1664B 

allows use of alternate extraction 

techniques, such as solid phase 

extraction (SPE) some discharges or 

waste streams may not be amenable to 

SPE. For these samples, 1664B should 

be applied as written. Conditioning of 

the solid-phase disk or device with 

solvents other than n-hexane (e.g., 

alcohol, acetone, etc) is allowed, only if 

this solvent(s) is completely removed 

from the SPE disk or device prior to 

passing the sample through the SPE disk 

or device. 

2. EPA is proposing to include in 

Table IB new EPA Method 200.5 and 

clarifying that the axial orientation of 

the torch is allowed for use with EPA 

Method 200.7. EPA Method 200.5 

‘‘Determination of Trace Elements in 

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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). It also includes 

performance data for the axial 

configuration that is not in Method 

200.7 because the axial technology torch 

results were not available when Method 

200.7 was developed. For some 

elements the axial orientation results in 

greater sensitivity and lower detection 

limits than the radial orientation. EPA 

now authorizes the use of Method 200.5 

in testing under its Safe Drinking Water 

Act Program (73 FR 31616, June 6, 

2008). Approval of Method 200.5 and 

the flexibility within Method 200.7 will 

allow laboratories to use either axial 

instruments or radial instruments to 

measure metals in water samples. 

3. EPA is proposing to add EPA 

Method 525.2, an updated version of 

EPA Method 525.1, in Table IG (Test 

Methods for Pesticide Active 

Ingredients) as an additional approved 

method for all parameters for which 

EPA has previously approved Method 

525.1. Further, EPA is soliciting 

comment on whether EPA should 

substitute Method 525.2 for Method 

525.1. 

EPA is proposing to include Pesticide 

Methods from Table IG in Table ID (Test 

Procedures for Pesticides). Specifically, 

EPA is proposing to add EPA Method 

525.2 for the same pesticides for which 

EPA has approved Method 525.1 in 

Table IG. Both methods use GC/MS 

methodology. 

EPA is proposing to add some of the 

Pesticide Active Ingredients methods in 

Table IG that have been in use for more 

than 10 years to Table ID for general 

use. These methods are: 

a. EPA Method 608.1, ‘‘The 

Determination of Organochloride 

Pesticides in Municipal and Industrial 

Wastewater.’’ This is a gas 

chromatographic (GC) method used to 

determine certain organochlorine 

pesticide compounds listed in industrial 

and municipal discharges. 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 is a GC 

method used to determine certain 

organochlorine pesticides compounds 

in industrial and municipal discharges. 

This method measures chlorothalonil, 

DCPA, dichloran, methoxychlor, and 

permethrin. 

c. EPA Method 614, ‘‘The 

Determination of Organophosphorus 

Pesticides in Municipal and Industrial 

Wastewater.’’ This is a GC method used 

to determine organophosphorus 

compounds in industrial and municipal 

discharges. This method measures 

azinphos methyl, demeton, diazinon, 

disulfoton, ethion, malathion, parthion 

methyl, and parathion ethyl. 

d. EPA Method 614.1, ‘‘The 

Determination of Organophosphorus 

Pesticides in Municipal and Industrial 

Wastewater.’’ This is a GC method used 

to determine organophosphorus 

compounds in industrial and municipal 

discharges. This method measures 

dioxathion, EPN, ethion, and terbufos. 

e. EPA Method 615, ‘‘The 

Determination of Chlorinated 

Herbicides in Municipal and Industrial 

Wastewater.’’ This is a GC method used 

to determine chlorinated herbicides 

compounds in industrial and municipal 

discharges. 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 is a GC 

method used to determine organohalide 

compounds in industrial and municipal 

discharges. This method measures 

aldrin, a-BHC, b-BHC, g-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 is a GC method used to determine 

triazine pesticides compounds in 

industrial and municipal discharges. 

This method measures ametryn, atraton, 

atrazine, prometon, prometryn, 

propazine, sec-bumeton, simetryn, 

simazine, terbuthylazine, terbutryn. 

h. EPA Method 622, ‘‘The 

Determination of Organophosphorus 

Pesticides in Municipal and Industrial 

Wastewater.’’ This is a GC method used 

to determine organophosphorus 

pesticides compounds in industrial and 

municipal discharges. 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 is a GC method used 

to determine thiophosphate pesticides 

compounds in municipal and industrial 

discharges. 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 is a high-performance 

liquid chromatographic (HPLC) method 

used to determine carbamate and urea 

pesticide compounds in industrial and 

municipal discharges. This method 

measures aminocarb, barban, carbaryl, 

carbofuran, chlorpropham, diuron, 

fenuron, fenuron-TCA, fluometuron, 

linuron, methiocarb, methomyl, 

mexacarbate, monuron, neburon, 

oxamyl, propham, propoxur, siduron, 

swep. 

4. EPA is proposing to add in Table 

IC EPA 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. 

These ethers are used in brominated 

flame retardants. This method uses 

isotope dilution and internal standard 

high resolution gas chromatography/ 

high resolution mass spectrometry 

(HRGC/HRMS). This method allows use 

of a temperature-programmed injector/ 

vaporizer and a short column to 

improve recoveries of the octa-, nona-, 

and decabrominated diphenyl ethers. 

5. EPA is proposing to add in Table 

IC EPA Method 1668C, ‘‘Chlorinated 

Biphenyl Congeners in Water, Soil, 

Sediment, Biosolids, and Tissue by 

HRGC/HRMS.’’ This method determines 

individual chlorinated biphenyl 

congeners in environmental samples by 

isotope dilution and internal standard 

high resolution gas chromatography/ 

high resolution mass spectrometry 

(HRGC/HRMS). Current Part 136 

methods only measure a mixture of 

congeners in seven Aroclors—PCB– 

1016, PCB–1221, PCB–1232, PCB–1242, 

PCB–1248, PCB–1254, and PCB–1260. 

EPA Method 1668C can measure the 209 

individual PCB congeners in these 

mixtures. EPA developed Method 1668 

for use in wastewater, surface water, 

soil, sediment, biosolids, and tissue 

matrices. 

EPA first published Method 1668 in 

1999 and it is being used in several 

environmental applications, including 

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58028 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

NPDES permits. EPA based today’s 

proposed version, 1668C, on the results 

of an interlaboratory validation study 

(EPA 2010a, b), peer reviews (EPA 

2010c), and user experiences. In the 

development and subsequent multilaboratory validation of this method, 

EPA has evaluated method performance 

characteristics, such as selectivity, 

calibration, bias, precision, quantitation 

and detection limits. For example, EPA 

has observed that detection limits and 

quantitation levels are usually 

dependent on the level of interferences 

and laboratory background levels rather 

than instrumental limitations. Thus, the 

published minimum levels of 

quantitation are conservative estimates 

of the concentrations at which a 

congener can be measured with 

laboratory contamination present (EPA 

2010d). 

EPA recognizes that the performance 

of this Method may vary among the 209 

congeners, and in different matrices. 

This is typical of multi-analyte methods 

because not all chemicals respond 

identically to extraction and clean up 

techniques, or have identical instrument 

responses. 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 a 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 PCB method and the 

polybrominated diphenyl ether (PBDE) 

Method 1614A are performance-based 

methods. This means that users have the 

flexibility to modify the method to 

adapt to the sometimes unique 

characteristics of the user’s sample. 

There is flexibility to modify the sample 

preparation steps to remove substances 

that interfere with measurement of the 

PCB congeners. A consequence of this 

flexibility is that, after customizing a 

performance-based method for a specific 

sample or application, the user should 

continue to use the same customized 

procedures on these samples or 

applications to maintain data 

comparability. 

EPA Method 1668C, the 

interlaboratory study report, and peer 

reviews are in the docket for today’s 

rule and on EPA’s CWA methods Web 

site at http://www.epa.gov/

waterscience/methods. EPA lists 

Method 1668C in Table IC as the 

parameter, ‘‘PCBs 209 Congeners.’’ 

6. EPA is proposing to update in 

Table IH EPA Method 1622, 

‘‘Cryptosporidium in Water by 

Filtration/IMS/FA’’ and EPA Method 

1623, ‘‘Cryptosporidium and Giardia in 

Water by Filtration/IMS/FA’’ to reflect 

changes made in the December 2005 

versions of these methods. EPA’s 

drinking water program uses the 2005 

versions of the methods. The methods 

allow the flexibility to choose among 

several types of filters, quality controls, 

and stains, as well as clarification on 

measuring sample temperatures, quality 

control sample requirements and use of 

quality control sample results, 

minimizing carry-over debris, analyst 

verification procedures and sample 

condition criteria upon receipt. This 

method substitution necessitates a 

change in the holding temperature 

(Table II) for Cryptosporidium and 

Giardia from 0–8 °C to refrigerate 

between 1–10 °C. 

7. EPA is proposing in Table IH 

revised versions of EPA Methods 

1103.1, 1106.1, 1600 (also in Table IA), 

1603, and 1680 to correct technical 

errors. Specifically, for Methods 1103.1 

and 1603, tryptone broth should be 

tryptone water (section 12.4.3). In 

addition, in Tables 2 and 3, 

respectively, of these two methods, the 

positive control organism for the 

cytochrome oxidase reagent has been 

changed to P. aeruginosa from E. 

faecalis, and the negative control 

organism for Simmons citrate agar has 

been changed to S. flexneri from E. coli 

for more definitive results. In section 

7.5.2 of Method 1603, the formula for 

magnesium chloride hexahydrate 

should have a dot before the waters 

rather than an alpha sign (MgCl2·6H2O). 

In Methods 1106.1 and 1600, in Tables 

6 and 7, respectively, the true spiked 

Enterococci ‘‘T (CFU/100 mL)’’ in the 

spiked sample based on the lot mean 

valued provided by the manufacturer 

should be 32 instead of 11.2. In Method 

1680, the lactose for Lauryl Tryptose 

Broth (LTB) should be 5.0 g, not 25.0 g 

(section 7.6.1), and the dipotassium 

hydrogen phosphate for EC medium 

should be 4.0 g, not 44.0 g (section 

7.7.1). 

8. EPA is proposing to add Method 

1627, ‘‘Kinetic Test Method for the 

Prediction of Mine Drainage Quality.’’ 

The method is a standardized simulated 

weathering test that provides 

information to predict the quality of 

mine drainage from coal mining 

operations or weathering. The method 

also can be a tool with which to 

generate data in the design and 

implementation of best management 

practices and treatment processes 

needed by mining operations to meet 

U.S. EPA discharge requirements at 40 

CFR part 434. Other publications have 

referred to this method generically as 

the ADTI Weathering Procedure 2 

(ADTI–WP2). EPA lists Method 1627 in 

Table IB as ‘‘Acid Mine Drainage.’’ The 

method is suitable for determinations of 

probable hydrologic consequences and 

to develop cumulative hydrologic 

impact assessment data to support 

Surface Mining Control and 

Reclamation Act (SMCRA) permit 

application requirements. Although this 

method is directed toward the coal 

mining industry and regulatory 

agencies, the method may be applicable 

to highway and other construction 

involving cut and fill of potentially 

acid-producing rock. This method may 

be used to predict the water quality 

characteristics (e.g., pH, acidity, metals) 

of mine site discharges using 

observations from sample behavior 

under simulated and controlled 

weathering conditions. The method was 

developed and evaluated in single, 

multiple and interlaboratory method 

validation studies in laboratories 

representing the mining industry, 

private sector, federal agencies, and 

academia. 

9. EPA proposes to approve EPA 

Method 624, ‘‘Purgeables,’’ for definitive 

measurements of acrolein and 

acrylonitrile in wastewater. Currently 

this method is approved only to screen 

samples for the presence of acrolein and 

acrylonitrile. Footnote 4 to Table IC 

requires that the analyst confirm 

occurrences with either EPA Method 

603 or 1624 because, when EPA 

promulgated this method, EPA believed 

the confirmatory step was necessary. 

Commenters on a previous proposed 

rule to amend part 136 (69 FR 18166, 

April 6, 2004) requested that EPA allow 

use of Method 624 for definitive 

determination of acrolein and 

acrylonitrile in wastewater without a 

confirmatory step and provided EPA 

with data. EPA has considered this 

comment and after reviewing additional 

data (Test America 1, 2) is proposing to 

revise the listing of Method 624 in Table 

IC to remove footnote 4 that requires a 

confirmatory analysis. 

B. Changes to 40 CFR 136.3 To Include 

New Standard Methods and New 

Versions of Approved Standard 

Methods 

EPA is proposing to revise how we 

identify approved methods that are 

published by the Standard Methods 

Committee. Currently in the tables at 

136.3(a), EPA lists these methods in one 

or more columns as being in the 18th, 

19th, 20th printed compendiums, or in 

the On-line editions published by the 

Standard Methods Committee. EPA 

identifies which versions are approved 

by the printed edition in which the 

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method is published or, in the case of 

the electronic version of the method, by 

the last two digits of the year in which 

the method was published by the 

Standard Methods Committee (e.g., 

Standard Method 2320 B–97). In some 

cases, EPA has approved more than one 

version of a Standard Method. Approval 

of several versions of the same Standard 

Method has led to inconsistencies in 

how laboratories conduct these analyses 

especially in quality assurance/quality 

control (QA/QC) practices. For this 

reason, EPA is proposing to approve 

only the most recent version of a 

method published by the Standard 

Methods Committee with as few 

exceptions as possible by listing only 

one version of the method with the year 

of publication designated by the last 

four digits in the method number (e.g., 

Standard Method 2320 B–1997). This 

change allows use of a specific method 

in any edition that includes a method 

with the same method number and year 

of publication. Previously, a laboratory 

only could use the method that was 

published in the edition of Standard 

Methods listed in the tables at 136.3(a). 

In some cases, EPA used footnotes to 

designate approved Standard Methods 

that are no longer published in 

Standard Methods. 

In addition, EPA is proposing to 

approve new Standard Methods, SM, 

new versions of currently approved SM, 

and the use of an already approved SM 

for a chemical that is not currently 

listed in Table IB. The new versions of 

currently approved SM have been 

revised to clarify or improve the 

instructions in the method, improve the 

quality control (QC) instructions, or 

make editorial corrections. The 

proposed new SM and new versions of 

SM are described in the following 

paragraphs. 

1. EPA is proposing to add SM 5520 

B–2001 and SM 5520 F–2001 for Oil 

and Grease determinations. These 

methods measure hexane extractable 

material (HEM). EPA is proposing these 

methods because they use n-hexane as 

the extraction solvent. EPA is not 

proposing SM 5520 G–2001 because it 

allows use of a co-solvent, such as 

acetone. In the preceding description of 

EPA’s proposed Method 1664B, EPA 

explained that oil and grease is a 

measurement defined by the solvent, in 

this case n-hexane, used to extract oil 

and grease from the sample. Thus, use 

of any other solvent system, such as a 

co-solvent is precluded. 

2. EPA is proposing to add SM 4500– 

NH3 G–1997, Ammonia (as N) and TKN, 

Phenate Method, which is an automated 

version of the previous version of a 

previously approved SM 4500–NH3

F–1997. 

3. EPA is proposing to add SM 

4500–B B–2000, Boron, Curcumin 

Method, which uses the same chemistry 

and instruments as Method I–3112–85. 

4. EPA is proposing to add SM 4140– 

1997, Inorganic Ions (Bromide, 

Chloride, Fluoride, Orthophosphate, 

and Sulfate), Capillary Ion 

Electrophoresis with Indirect UV 

Detection, which uses the same 

technology as the EPA approved ASTM 

Method D6508–00. 

5. EPA is proposing to add SM 3114 

C–2009, Arsenic and Selenium by 

Continuous Hydride Generation/Atomic 

Absorption Spectrometry, which is an 

automated version of the approved 

manual method, and uses the same 

technology as Method I–2062–85. 

6. EPA is proposing to add SM 3111 

E–1999 for determinations of aluminum 

and beryllium. The method uses the 

same instrumental techniques as SM 

3111D with an additional chelation 

concentration step for increased 

sensitivity. 

7. EPA is proposing to add SM 5220 

B–1997 for Chemical Oxygen Demand 

which is similar to EPA Method 410.3. 

8. EPA is proposing to add SM 4500 

NORG D–1997 for determinations of 

Kjeldahl Nitrogen—Total, which has a 

similar chemical and instrument setup 

as in EPA Method 351.2 in Table IB. 

The same chemical reaction is measured 

in both of these methods. 

9. EPA is proposing to add SM 4500 

P G–1999 and SM 4500 P H–1999, 

Phosphorus. Both of these methods use 

separate flow injection instrumentation 

that is the same as EPA Method 365.1. 

10. EPA is proposing to add SM 4500 

P E–1999 and SM 4500 P F–1999, 

Phosphorus. These methods, 4500 P 

E–1999 Manual Single Reagent and 

F–1999 Automated Ascorbic Acid, have 

been approved for drinking water 

analyses (73 FR 31616, June 3, 2008). 

11. EPA is proposing to add SM 4500 

O B, D, E and F–2001, Oxygen, 

Iodometric Methods. EPA is proposing 

these methods because Standard 

Methods has broken down the Winkler 

titration method into several sections. 

Sections 4500 O B, D, E and F have been 

added to provide a more detailed 

Winkler titration. Section B contains 

information on how to collect the 

sample and what pretreatment may be 

needed for just the Winkler titrations. 

Sections D, E, and F contain specific 

sample pretreatment for interferences. 

Section D (see Item 12) is for ferrous 

iron interferences. Section E (see Item 

13) is for samples with a high 

concentration of Total Suspended 

Solids. Section F is for samples with 

large concentrations of biological solids. 

These sections are similar to the 

instructions in ASTM D888, AOAC 

973.45, and USGS I–1575–78. 

12. EPA is proposing to add SM 4500 

O D–2001, Oxygen, Permanganate 

Modification. This method for 

determinations of dissolved oxygen 

contains the same permanganate 

pretreatment step that is specified in 

ASTM D 888 and AOAC 973.45. 

13. EPA is proposing to add SM 4500 

O E–2001, Oxygen, Alum Flocculation 

Modification. This method for dissolved 

oxygen describes a pretreatment step 

that removes high concentrations of 

suspended solids. 

14. EPA is proposing to add SM 3500 

K C–1997, Potassium, Selective 

Electrode Method. This method uses the 

same electrochemical procedure to 

measure Potassium that is used in the 

Standard Methods for ammonia, 

chloride, cyanide, and nitrate. Only the 

electrode construction is different. 

15. EPA is proposing to add SM 2540 

E–1997 for determinations of 

Residues—Volatile. This fixed and 

volatile solids method uses the same 

equipment and procedures to measure 

this method defined parameter as 

approved EPA Method 160.4. 

16. EPA is proposing to add SM 4500 

SiO2 E–1997 and SM 4500 SiO2 F–1997, 

Silica. These methods have the same 

instrument setup and molybdate color 

reagent as USGS Method I–2700, but 

utilize different reducing agents to 

produce molybdenum blue color. There 

are slight modifications in the chemical 

reaction, but the molybdenum blue final 

analyte is the same. 

17. EPA is proposing to add SM 4500 

SO4 C–1997, D–1997, E–1997, F–1997 

and G–1997, Sulfate. EPA is proposing 

to approve the online version of these 

methods because they are identical to 

the approved versions published in the 

18th, 19th and 20th edition of Standard 

Methods. EPA approved the online 

versions for drinking water use (73 FR 

31616, June 3, 2008). 

18. EPA is proposing to add SM 4500 

S2¥B–2000 and C–2000, Sulfide. These 

approved methods have been revised to 

describe more completely the sample 

collection, transportation and analysis 

steps. 

C. Changes to 40 CFR 136.3 To Include 

New ASTM Methods and New Versions 

of Previously Approved ASTM Methods 

EPA is proposing to add to the list of 

approved testing procedures new ASTM 

methods for existing pollutants in Table 

IB, such as cyanide, and methods for 

new pollutants, such as the 

nonylphenols in Table IC. EPA also is 

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58030 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

proposing new versions of previously 

approved ASTM methods. 

1. EPA is proposing to add ASTM 

D2036–09 Standard Test Methods for 

Cyanides in Water, Test Method A Total 

Cyanide after Distillation. In 2009, 

ASTM revised the version of this 

method currently listed in part 136. The 

method measures cyanides that are free, 

and strong-metal-cyanide complexes 

(e.g. iron cyanides) that dissociate and 

release free cyanide when refluxed 

under strongly acidic conditions. The 

cyanide in some cyano complexes of 

transition metals, for example, cobalt, 

gold, platinum, etc., is not determined. 

Samples are digested with sulfuric acid 

in the presence of magnesium chloride 

in a distillation reaction vessel that 

consists of a 1–L round bottom flask, 

with provision for an inlet tube and a 

condenser connected to a vacuum-type 

absorber. The flask is heated with an 

electric heater. Smaller distillation tubes 

such as 50-mL midi tubes or 6-mL 

MicroDistTM tubes described in D7284– 

08 can be used if the quality control 

requirements in D2036–09 are satisfied. 

After distillation, the cyanide 

concentration can be determined with 

titration, ion chromatography, 

colorimetric procedure 

(spectrophotometric), selective ion 

electrode, or flow injection analysis 

with gas diffusion separation and 

amperometric detection. The inclusion 

of ion chromatography and gas diffusion 

separation with amperometric detection 

as determinative steps (D2036–09, 

sections 16.5 and 16.6) will give users 

additional options to measure cyanide 

after distillation. Furthermore, these 

determinative steps can be used to 

mitigate interferences that have been 

associated with conventional 

colorimetric test methods. 

2. EPA is proposing to add ASTM 

D6888–09 Standard Test Method for 

Available Cyanide with Ligand 

Displacement and Flow Injection 

Analysis (FIA) Utilizing Gas Diffusion 

Separation and Amperometric 

Detection. This method is used to 

determine the concentration of available 

inorganic cyanide in an aqueous 

wastewater or effluent. The method 

detects the cyanides that are free and 

metal-cyanide complexes that are easily 

dissociated into free cyanide ions. The 

method does not detect the less toxic 

strong metal-cyanide complexes, 

cyanides that are not ‘‘amenable to 

chlorination.’’ Total cyanide can be 

determined for samples that have been 

distilled as described in Test Methods 

D2036–09, Test Method A, Total 

Cyanides after Distillation. Complex 

cyanides bound with nickel or mercury 

are released by ligand displacement 

with the addition of a ligand 

displacement agent prior to analysis. 

Other available cyanide species do not 

require ligand displacement under the 

test conditions. If samples are distilled 

for total cyanide, ligand exchange 

reagents are not required since the 

cyanide complexes are dissociated and 

absorbed into the sodium hydroxide 

capture solution during distillation. The 

treated or distilled sample is introduced 

into a flow injection analysis (FIA) 

system where it is acidified to form 

hydrogen cyanide. The hydrogen 

cyanide gas diffuses through a 

hydrophobic gas diffusion membrane, 

from the acidic donor stream into an 

alkaline acceptor stream. Up to 50-mg/ 

L sulfide is removed during flow 

injection to mitigate sulfide 

interference. The captured cyanide is 

sent to an amperometric flow cell 

detector with a silver-working electrode. 

In the presence of cyanide, silver in the 

working electrode is oxidized at the 

applied potential. The anodic current 

measured is proportional to the 

concentration of cyanide in the standard 

or sample injected. 

3. EPA is proposing to add 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. This 

method determines the concentration of 

total cyanide in wastewater, and detects 

the cyanides that are free and strongmetal-cyanide complexes (e.g., iron 

cyanides) that dissociate and release 

free cyanide when refluxed under 

strongly acidic conditions. This method 

has a range of approximately 2 to 400 

μg/L (parts per billion) total cyanide. 

Higher concentrations can be measured 

with sample dilution or lower injection 

volume. The determinative step of this 

method utilizes flow injection with 

amperometric detection based on ASTM 

D6888–09. Sample distillation is based 

on Lachat QuikChem Method 10–204– 

00–1–X. Prior to analysis, samples must 

be distilled with a micro-distillation 

apparatus described in the test method 

or with a suitable cyanide distillation 

apparatus specified in Test Methods D 

2036–09. The samples are distilled with 

a strong acid in the presence of 

magnesium chloride catalyst and 

captured in sodium hydroxide absorber 

solution. The absorber solution from the 

distillation is introduced into a flow 

injection analysis (FIA) system where it 

is acidified to form hydrogen cyanide. 

The hydrogen cyanide gas diffuses 

through a hydrophobic gas diffusion 

membrane, from the acidic donor stream 

into an alkaline acceptor stream. The 

captured cyanide is sent to an 

amperometric flow cell detector with a 

silver-working electrode. In the 

presence of cyanide, silver in the 

working electrode is oxidized at the 

applied potential. The anodic current 

measured is proportional to the 

concentration of cyanide. This method 

has been shown to be less susceptible to 

interferences compared to conventional 

spectrophotometric determinations for 

total cyanide. 

4. EPA is proposing to add ASTM 

D7511–09e2 Standard Test Method for 

Total Cyanide by Segmented Flow 

Injection Analysis, In-Line Ultraviolet 

Digestion and Amperometric Detection. 

This method determines the 

concentration of total cyanide in 

drinking and surface waters, as well as 

domestic and industrial wastes. Cyanide 

ion (CN-), hydrogen cyanide in water 

(HCN(aq)), and the cyano-complexes of 

zinc, copper, cadmium, mercury, nickel, 

silver, and iron may be determined by 

this method. Cyanide ions from Au(I), 

Co(III), Pd(II), and Ru(II) complexes are 

only partially determined. The 

applicable range of the method is 3 to 

500 μg/L cyanide using a 200-μL sample 

loop. The range can be extended to 

analyze higher concentrations by 

sample dilution or by changing the 

sample loop volume. ASTM D7511– 

09e2 decomposes complex cyanides by 

narrow band, low watt UV irradiation in 

a continuously flowing acidic stream at 

room temperature. Reducing and 

complexing reagents, combined with the 

room temperature narrow band low watt 

UV, minimize interferences. The 

hydrogen cyanide generated passes 

through a hydrophobic membrane into a 

basic carrier stream. The cyanide 

concentration is determined by 

amperometry. This method operates 

similarly to available cyanide methods 

OIA1677 and ASTM D6888–09. The 

available cyanide methods employ a 

preliminary ligand addition to liberate 

cyanide ion from weak to moderate 

metal cyanide complexes. These 

available cyanide methods were 

developed because they overcome 

significant interferences caused by the 

preliminary chlorination and/or 

distillation processes. Instead of ligands, 

ASTM D7511–09e2 irradiates the 

sample causing strong metal cyanide 

complexes plus all complexes measured 

by the available cyanide methods to 

liberate cyanide and generate hydrogen 

cyanide. Once the sample solution 

passes from the UV irradiation, the 

measurement principle is equivalent to 

OIA1677 and/or ASTM D6888–09. 

5. Because there were no EPAapproved methods for free cyanide 

when water quality criteria were 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58031 

established for free cyanide EPA 

recommended measurement of cyanide 

after a ‘‘total’’ distillation. Analytical 

methods for free cyanide have been 

developed, and in today’s rule EPA is 

proposing to add free cyanide as a 

parameter (24A in Table IB.) For 

determinations of this parameter, EPA is 

proposing to allow use of the approved 

available cyanide method, OIA 1677–09, 

and two ASTM methods (D4282–02 and 

D7237–10.) ASTM D4282–02 Standard 

Test Method for Determination of Free 

Cyanide in Water and Wastewater by 

Microdiffusion determines free cyanide 

as the cyanide that diffuses into a 

sodium hydroxide solution from a 

solution at pH 6. It is not applicable to 

cyanide complexes that resist 

dissociation, such as hexacyanoferrates 

and gold cyanide, and it does not 

include thiocyanate and cyanohydrin. 

ASTM D7237–10 Standard Test Method 

for Free Cyanide with Flow Injection 

Analysis (FIA) Utilizing Gas Diffusion 

Separation and Amperometric Detection 

determines free cyanide with the same 

instrumentation and technology as 

approved methods, ASTM D6888–09 

and OIA 1677–09, but under milder 

(less acidic) conditions and without use 

of ligand replacement reagents. 

6. EPA is proposing to add ASTM 

D888–09 Standard Test Method for 

Dissolved Oxygen in Water. This 

method determines dissolved oxygen 

concentrations in water using the 

titrimetric (Part A), polarographic (Part 

B) and luminescence-based (Part C) 

detection methods. This standard test 

method is applicable to the 

determination of dissolved oxygen 

between 0.05–20 ppm in influent, 

effluent or ambient water testing. ASTM 

recently updated Part C of this method 

to include a detailed description of the 

technology and to update calibration 

procedures to include a two-point 

calibration and an air saturated water 

calibration in addition to a water 

saturated air calibration. This method 

may be used for Biological Oxygen 

Demand (BOD) and Carbonaceous 

Oxygen Demand (CBOD.) 

7. EPA is proposing to add ASTM 

D7573–09 Standard Test Method for 

Total Carbon and Organic Carbon in 

Water by High Temperature Catalytic 

Combustion and Infrared Detection. 

This Method has the same chemical and 

instrument setup as approved SM 5310 

B–2000. 

8. EPA is proposing to add in Table 

IC ASTM D7065–06: Standard Test 

Method for Determination of five 

chemicals: Nonylphenol (NP), 

Bisphenol A (BPA), p-tert-Octylphenol 

(OP), Nonylphenol Monoethoxylate 

(NP1EO), and Nonylphenol 

Diethoxylate (NP2EO) in Environmental 

Waters by Gas Chromatography Mass 

Spectrometry. These five chemicals are 

partitioned into an organic solvent, 

separated using gas chromatography and 

detected with mass selective detection. 

These chemicals or isomer mixtures are 

qualitatively and quantitatively 

determined. Although this method 

adheres to selected ion monitoring mass 

spectrometry, full scan mass 

spectrometry has also been shown to 

work well under these conditions. This 

method has been multi-laboratory 

validated for use with surface water and 

waste treatment effluent samples and is 

applicable to these matrices. It has not 

been investigated for use with salt water 

or solid sample matrices. The reporting 

limit for nonylphenol is 5 μg/L (ppb); 

the chronic Freshwater Aquatic Life 

Ambient Water Quality Criterion is 6.6 

ppb. 

9. EPA is proposing to add in Table 

IC ASTM D7574–09: Standard Test 

Method for Determination of BPA in 

Environmental Waters by Liquid 

Chromatography/Tandem Mass 

Spectrometry. BPA is an organic 

chemical produced in large quantities. 

BPA is soluble in water and undergoes 

degradation in the environment. The 

reporting limit for BPA is 20 ng/L which 

is fifty times less than the limit in 

D7065–06 (see preceding Item 8). The 

method is based on a solid phase 

extraction (SPE) followed by separation 

with liquid chromatography and tandem 

mass spectrometry (LC/MS/MS), which 

reduces the amount of sample required, 

solvents, the analysis time, and the 

reporting limits. The method has been 

tested in effluents from secondary and 

tertiary publicly owned treatment works 

(POTW), and fresh surface and ground 

water. 

10. EPA is proposing to add in Table 

IC ASTM D7485–09: Standard Test 

Method for Determination of NP, OP, 

NP1EO, and NP2EO in Environmental 

Waters by Liquid Chromatography/ 

Tandem Mass Spectrometry. The 

method extracts these four chemicals 

from water with SPE followed by 

LC/MS/MS separation and detection. 

These chemicals are qualitatively and 

quantitatively determined by this 

method. This method uses single 

reaction monitoring (SRM) mass 

spectrometry. Environmental waters 

tested using this method were sewage 

treatment plant effluent, river water, 

seawater, and a modified ASTM D5905 

artificial wastewater. The reporting limit 

for nonylphenol is 100 ng/L, ppt. The 

Freshwater and Saltwater Aquatic Life 

Ambient acute criterion is 7.0 ppb, and 

the chronic criterion is 1.7 ppb. 

11. EPA is not proposing to include in 

Table IB two ASTM oil and grease 

methods, D7066–04 and D7575–10 

because neither method uses n-hexane 

to determine oil and grease as hexane 

extractable material (HEM). As 

previously explained in the discussion 

of Method 1664B, HEM is a 

measurement defined by the solvent (nhexane) used to extract oil and grease 

from the sample. D7066–04 employs a 

proprietary solvent, S–316, a dimer/ 

trimer of chlorotrifluoroethylene to 

measure S–316-extractable substances 

from an acidified sample. Method 

D7066 may be useful for determinations 

of total petroleum hydrocarbons (TPH). 

Although TPH has been measured in 

some applications, EPA has never 

included it as a Part 136 pollutant nor 

received any convincing evidence that it 

should do so. Although S–316 is not the 

same solvent as the fluorocarbon, 

Freon®, it is a fluorochlorohydrocarbon. 

Instead of n-hexane, ASTM D7575–10 

uses a different extracting process, an 

extracting membrane, followed by 

infrared measurement of the materials 

in the sample that can pass through the 

membrane. Several other steps in 

D7575–10 significantly differ from 1664 

including: Use of 10-mL sample aliquot 

from sample bottle vs. entire contents of 

1–L sample; homogenization of samples; 

and the challenge of pushing solid oil 

and grease samples through a 

membrane. The results of a multilaboratory study (OSS 2009) that the 

developer conducted as part of ASTM’s 

evaluation of D7575 are in the docket. 

D. Changes to 40 CFR 136.3 To Include 

Alternate Test Procedures 

To promote method innovation, EPA 

maintains a program whereby method 

developers may apply for an EPA 

review and potentially for approval of 

alternate test procedures. This Alternate 

Test Procedure (ATP) program is 

described for Clean Water Act 

applications at Parts 136.4 and 136.5. 

EPA has reviewed and is proposing for 

nationwide use eight alternate test 

procedures. These proposed new 

methods include: Hach Company’s 

Method 10360 Luminescence 

Measurement of Dissolved Oxygen 

(LDO®) in Water, In-Situ Incorporated’s 

Method 1002–8–2009 Dissolved Oxygen 

(DO) Measurement by Optical Probe, 

Method 1003–8–2009 Biochemical 

Oxygen Demand (BOD) Measurement by 

Optical Probe, and Method 1004–8– 

2009 Carbonaceous Biochemical Oxygen 

Demand (CBOD) Measurement by 

Optical Probe August 2009, Mitchell 

Method M5271 and M5331 for 

measuring turbidity in wastewater; 

Thermo Scientific’s Orion Method 

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AQ4500 for measuring turbidity in 

wastewater; and Systea Scientific, LLC’s 

Systea Easy (1-Reagent) Nitrate Method. 

Descriptions of these new methods 

included for approval are as follows: 

1. EPA is proposing to approve Hach 

Company’s Method 10360 

Luminescence Measurement of 

Dissolved Oxygen (LDO®) in 

wastewater, Revision 1.1 dated January 

4, 2006. EPA has reviewed this method 

and the data generated in a multilaboratory validation study performed 

by Hach Company and is proposing to 

approve it for use in measuring 

dissolved oxygen. EPA is also proposing 

to approve the Hach method 10360 to be 

used for Dissolved Oxygen (DO) when 

determining BOD and CBOD. 

This method uses an optical probe to 

measure the light emission 

characteristics from a luminescencebased reaction that takes place at the 

sensor-water interface. A light emitting 

diode (LED) provides incident light 

required to excite the luminophore 

substrate. In the presence of dissolved 

oxygen, the reaction is suppressed. The 

resulting dynamic lifetime of the excited 

luminophore is evaluated and equated 

to DO concentration. 

The method involves the following 

steps: 

• Calibration of the probe using 

water-saturated air, and 

• Measurement of the dissolved 

oxygen in the sample using the probe. 

Approved methods for measuring 

dissolved oxygen are listed at 40 CFR 

136.3, Table IB. The performance 

characteristics of the Hach Company 

Method 10360 were compared to the 

characteristics of the methods listed at 

40 CFR 136.3, Table IB for measurement 

of dissolved oxygen. Because the Hach 

Company Method 10360 is equally 

effective relative to the methods already 

promulgated in the regulations, EPA is 

proposing to include this method in the 

list of methods approved for measuring 

dissolved oxygen concentrations in 

wastewater when determining BOD and 

CBOD. 

2. EPA is proposing to approve In-Situ 

Incorporated’s Method 1002–8–2009 

Dissolved Oxygen Measurement by 

Optical Probe. EPA has reviewed this 

method and the data generated in a 

multi-laboratory validation study 

performed by In-Situ Incorporated and 

is proposing to approve it for use in 

measuring dissolved oxygen. In-Situ 

Method 1002–8–2009 uses a new form 

of electrode based on the luminescence 

emission of a photoactive chemical 

compound and the quenching of that 

emission by oxygen to measure 

dissolved oxygen concentration. 

The method involves the following 

steps: 

• Calibration of the probe using 

water-saturated air, and 

• Measurement of the dissolved 

oxygen in the sample using the probe. 

Approved methods for measuring 

dissolved oxygen are listed at 40 CFR 

136.3, Table IB. The performance 

characteristics of the In Situ Method 

1002–8–2009 were compared to the 

characteristics of the methods listed at 

40 CFR 136.3, Table IB for measurement 

of dissolved oxygen. Because the In-Situ 

Method 1002–8–2009 is equally 

effective relative to the methods already 

promulgated in the regulations, EPA is 

proposing In-Situ Method 1002–8–2009 

for inclusion in the list of methods 

approved for measuring dissolved 

oxygen concentrations in wastewater. 

3. EPA is proposing to approve In-Situ 

Incorporated’s Method 1003–8–2009 

Biochemical Demand (BOD) 

Measurement by Optical Probe. EPA has 

reviewed this method and the data 

generated in a multi-laboratory 

validation study performed by In-Situ 

Incorporated and is proposing to 

approve it for measuring BOD. 

In-Situ Method 1003–8–2009 uses a 

new form of electrode based on the 

luminescence emission of a photoactive 

chemical compound and the quenching 

of that emission by oxygen to measure 

dissolved oxygen concentration when 

performing the 5-day BOD test. 

The method involves the following 

steps: 

• Filling a BOD bottle with diluted 

seeded sample, 

• Measuring the dissolved oxygen in 

the sample using an optical DO probe, 

• Sealing and incubating the bottle 

for five days, 

• Measuring the dissolved oxygen 

with an optical probe after the five day 

incubation period, and 

• Calculating the BOD from the 

difference between the initial and final 

dissolved oxygen measurements. 

Approved methods for measuring 

BOD are listed at 40 CFR 136.3, Table 

IB. The performance characteristics of 

In-Situ Method 1003–8–2009 were 

compared to the characteristics of the 

methods listed at 40 CFR 136.3, Table 

IB for measurement of BOD. Because InSitu Method 1003–8–2009 is equally 

effective relative to the methods already 

promulgated in the regulations, EPA is 

proposing In-Situ Method 1003–8–2009 

for inclusion in the list of methods 

approved for measuring BOD. 

4. EPA is proposing to approve In-Situ 

Incorporated’s Method 1004–8–2009 

Carbonaceous Biochemical Oxygen 

Demand (CBOD) Measurement by 

Optical Probe. EPA has reviewed this 

method and the data generated in a 

multi-laboratory validation study 

performed by In-Situ Incorporated and 

is proposing to approve it for use in 

measuring carbonaceous biochemical 

oxygen demand (CBOD). In-Situ Method 

1004–8–2009 uses a new form of 

electrode based on the luminescence 

emission of a photoactive chemical 

compound and the quenching of that 

emission by oxygen to measure 

dissolved oxygen concentration when 

performing the CBOD test. 

The method involves the following 

steps: 

• Filling a BOD bottle with diluted 

seeded sample, 

• Adding a chemical nitrification 

inhibitor, 

• Measuring the dissolved oxygen in 

the sample using an optical dissolved 

oxygen probe, 

• Sealing and incubating the bottle 

for five days, 

• Measuring the dissolved oxygen 

with an optical probe after the five day 

incubation period, and 

• Calculating the CBOD from the 

difference between the initial and final 

dissolved oxygen measurements. 

Approved methods for measuring 

CBOD are listed at 40 CFR 136.3, Table 

IB. The performance characteristics of In 

Situ-Method 1004–8–2009 were 

compared to the characteristics of the 

methods listed for measurement of 

CBOD. Because In-Situ Method 1004–8– 

2009 is equally effective relative to the 

methods already promulgated in the 

regulations, EPA is proposing In-Situ 

Method 1004–8–2009 for inclusion in 

the list of methods approved for 

measuring CBOD. 

5. EPA is proposing to approve the 

Mitchell Method M5271 dated July 31, 

2008. This method uses laser based 

nephelometry to measure turbidity in 

drinking water and wastewater. The 

method involves the following steps for 

instruments other than on-line 

continuous models: 

• Mixing the sample to thoroughly 

disperse the solids, 

• Waiting until air bubbles disappear, 

• Pouring a sample into a 

turbidimeter tube, and 

• Reading turbidity directly from the 

instrument scale or from the appropriate 

calibration curve. 

Approved methods for turbidity are 

listed at 40 CFR 136.3 Table 1B. The 

performance characteristics of Mitchell 

Method M5271 were compared to the 

performance characteristics of EPA 

Method 180.1 listed at 40 CFR 136.3 for 

measurement of turbidity. Comparisons 

were based on results obtained from 

turbidimeters placed in series which 

took measurements at one minute 

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intervals over a 20 to 30 hour time 

period at three different public water 

supply systems (in one case 

measurements were taken at 15 minute 

intervals). Testing included source 

water from one ground water source and 

two surface water sources and included 

at least one natural filter event (backflush) in lieu of artificially calibrated 

spikes using a primary standard spiking 

solution. Additionally, a demonstration 

of performance at higher turbidities was 

conducted by making replicate 

measurements of primary standards at 

four levels (5 NTU, 10 NTU, 20 NTU 

and 40 NTU). Results showed excellent 

correlation between measurements 

made using a tungsten filament 

incandescent bulb as specified in EPA 

Method 180.1 and those made using the 

laser light source specified in Mitchell 

Method M5271. Based on the results of 

these studies, EPA has determined that 

Mitchell Method M5271 is as effective 

as the methods already promulgated in 

the regulations. EPA is proposing to add 

this method to the list of methods 

approved for measurement of turbidity 

in wastewater. 

6. EPA is proposing Mitchell Method 

M5331 dated July 31, 2008. This method 

uses LED based nephelometry to 

measure turbidity. The method involves 

the following steps for instruments 

other than on-line continuous models: 

• Mixing the sample to thoroughly 

disperse the solids, 

• Waiting until air bubbles disappear, 

• Pouring the sample into 

turbidimeter tube, and 

• Reading turbidity directly from the 

instrument scale or from the appropriate 

calibration curve. 

Approved methods for turbidity are 

listed at 40 CFR 136.1 Table 1B. The 

performance characteristics of Mitchell 

Method 5331 were compared to the 

performance characteristics of EPA 

Method 180.1 listed at 40 CFR 136.3 for 

measurement of turbidity. Comparisons 

were based on results obtained from 

turbidimeters placed in series, which 

took measurements at one minute 

intervals over a 20 to 30 hour time 

period at three different public water 

supply systems (in one case 

measurements were taken at 15 minute 

intervals). Testing included source 

water from one ground water source and 

two surface water sources and included 

at least one natural filter event (backflush) in lieu of artificially calibrated 

spikes using a primary standard spiking 

solution. Additionally, a demonstration 

of performance at higher turbidities was 

conducted by making replicate 

measurements of primary standards at 

four levels (5 NTU, 10 NTU, 20 NTU 

and 40 NTU). Results showed excellent 

correlation between measurements 

made using a tungsten filament 

incandescent bulb as specified in EPA 

Method 180.1 and the LED light source 

specified in Mitchell Method M5331. 

Based on the results of these studies, 

EPA has determined that Mitchell 

Method M5331 is equally effective 

relative to the methods already 

promulgated in the regulations. EPA is 

proposing to add this method to the list 

of methods approved for measurement 

of turbidity in wastewater. 

7. EPA is proposing to approve 

Thermo Scientific’s Orion Method 

AQ4500 dated March 12, 2009. This 

method uses LED-based nephelometry 

to measure turbidity. The method 

involves the following steps: 

• Calibration of the instrument using 

a primary calibration standard, 

• Placing the sample into the sample 

chamber, and 

• Reading the turbidity result 

displayed on the instrument. 

Approved methods for turbidity are 

listed at 40 CFR 136.3 Table IB. The 

performance characteristics of Thermo 

Scientific’s Orion Method AQ4500 were 

compared to the performance 

characteristics of EPA Method 180.1 

listed at 40 CFR 136.3 for measurement 

of turbidity. Comparisons were based on 

an ASTM round robin study comparing 

results from analyses of 28 different 

samples of various types including 

formazin standards, styrene divinyl 

benzene (SDVB) co-polymer bead 

standards and real world samples 

ranging from approximately 2 NTU to 

over 1,000 NTU. These analyses were 

conducted using turbidimeters with 

various light sources including tungsten 

filament incandescent bulbs as specified 

in EPA Method 180.1 and white LEDs 

as specified in Thermo Scientific’s 

Orion Method AQ4500. Additionally, a 

demonstration of performance at lower 

turbidities was conducted by making 20 

replicate measurements of dilute 

formazin standards at four levels (0.2 

NTU, 0.5 NTU, 1 NTU, and 2 NTU) 

using turbidimeters with tungsten 

filament incandescent bulbs as specified 

in EPA Method 180.1 and turbidimeters 

using white LEDs as specified in 

Thermo Scientific Orion Method 

AQ4500. Results showed significant 

correlation between measurements 

made using a tungsten filament 

incandescent bulb as specified in EPA 

Method 180.1 and those made using the 

LED light source specified in Thermo 

Scientific’s Orion Method AQ4500. 

Based on the results of these studies, 

EPA has determined that Thermo 

Scientific’s Orion Method AQ4500 is as 

effective as the methods already 

promulgated in the regulations. EPA is 

proposing to add this method to the list 

of methods approved for measurement 

of turbidity in wastewater. 

8. EPA is proposing to approve Systea 

Scientific, LLC’s Systea Easy (1-Reagent) 

Nitrate Method dated February 4, 2009. 

This is a method that uses automated 

discrete analysis, and 

spectrophotometry to determine 

concentrations of nitrate and nitrite 

combined or singly. The method 

involves the following steps: 

• Reduction of nitrate in a sample to 

nitrite using a non-hazardous 

proprietary reagent, 

• Diazotizing the nitrite originally in 

the sample plus the reduced nitrate with 

sulfanilamide followed by coupling 

with N-(1-napthyl) ethylenediamine 

dihydrochloride under acidic 

conditions to form a highly colored azo 

dye, 

• Colorimetric determination in 

which the absorbance of color at 546 nm 

is directly proportional to the 

concentration of the nitrite plus the 

reduced nitrate in the sample, 

• Measurement of nitrite singly, if 

needed, by analysis of the sample while 

eliminating the reduction step, and 

• Subtraction of the nitrite value from 

that of the combined nitrate plus nitrite 

value to measure nitrate singly if 

needed. 

Approved methods for nitrate, nitrite 

and combined nitrate/nitrite are listed at 

40 CFR 136.3, Table 1B. The 

performance characteristics of the 

Systea Easy (1-Reagent) Nitrate Method 

were compared to the characteristics of 

the methods listed at 40 CFR 136.3 for 

nitrate and nitrite. Based on the results 

of the comparative studies, EPA has 

determined that the Systea Easy (1- 

Reagent) Nitrate Method is as effective 

as the methods already promulgated in 

the regulations for use in determining 

concentrations of nitrate and nitrite and 

combined nitrate/nitrite. The method is 

a ‘‘green’’ alternative to other approved 

methods that use cadmium, a known 

carcinogen, for the reduction of nitrate 

to nitrite. The performance of Systea 

Easy (1-Reagent) Nitrate Method is 

equivalent to other methods already 

approved for measurement of nitrate, 

nitrite and combined nitrate/nitrite in 

wastewater. 

E. Clarifications and Corrections to 

Previously Approved Methods in 40 CFR 

136.3 

EPA is proposing a clarification to 

procedures for measuring 

orthophosphate, and is proposing to 

correct typographical or other citation 

errors in part 136. 

1. EPA is clarifying the purpose of the 

immediate filtration requirement in 

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orthophosphate measurements, which 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. This filtration excludes any 

particulate forms of phosphorus that 

might hydrolyze into orthophosphorus 

in a slightly acidic sample during the 

allowed 48 hour holding time. Each grab 

sample must be filtered within 15 

minutes of collection to prevent 

orthophosphate formation. Specifically, 

filtration may not be delayed until the 

final grab sample is collected; each grab 

sample must be filtered upon collection. 

However, the filtered grab samples may 

be held for compositing up to the 

48-hour holding time. 

2. EPA is proposing to correct missing 

citations to the table of microbiological 

methods for ambient water monitoring 

which are specified in Table IH at 40 

CFR 136.3. Stakeholders asked EPA to 

separately specify the microbiological 

methods that EPA has approved for 

wastewater (Table IA) from those for 

ambient water. On August 15, 2005 

(70 FR 48256), EPA proposed to move 

microbial (bacterial and protozoan) 

methods which were applicable to 

ambient water to a new table, Table IH. 

However, in the final rule of March 26, 

2007 (72 FR 14220), EPA inadvertently 

omitted fecal coliform, total coliform, 

and fecal streptococcus methods from 

the table. EPA is proposing to add these 

methods to Table IH. 

3. EPA is proposing to correct several 

other typographical or minor citation 

errors, such as incomplete or incorrect 

method citations. 

F. Proposed Revisions in Table II at 40 

CFR 136.3(e) to Required Containers, 

Preservation Techniques, and Holding 

Times 

EPA is proposing revisions to Table II 

at 136.3(e) to clarify how to resolve 

conflicts between instructions in this 

table and instructions in an approved 

method or other source, and to amend 

some of the current requirements in 

Table II. 

1. The introductory text to Table II at 

136.3(e) specifies that the instructions 

in the table take precedence over other 

sources of this information. EPA 

publishes holding time and related 

instructions in Table II to provide a 

consistent set of instructions, and for 

other reasons. Not all methods contain 

complete instructions, and some 

otherwise equivalent methods (or 

methods for the same parameter) have 

conflicting instructions. For example, 

Table II instructions specify the 48 hour 

BOD holding time while some Part 136 

methods recommend 24 hours. In this 

instance Table II instructions take 

precedence. EPA recognizes that there 

may be cases where new technologies or 

advancements in current technologies 

may produce approved methods with 

instructions for a specific parameter that 

differ from Table II instructions, and 

provide better results. Cyanide 

determinations and some automated 

methods may fall into this category. 

Therefore, EPA is proposing to revise 

the text at 136.3(e) to allow a party to 

submit documentation to their 

permitting or other authority that 

supports use of an alternative approach. 

EPA is proposing to revise the 

introductory text to the table to read as 

follows: ‘‘Information in this table takes 

precedence over instructions provided 

in specific methods or elsewhere unless 

a party documents the acceptability of 

an alternative to the Table II 

instructions. The nature, timing and 

extent of the required documentation 

(i.e. how to apply and review as well as 

the amount of supporting data) are left 

to the discretion of the permitting 

authority (State Agency or EPA Region) 

or other authority and may rely on 

instructions, such as those provided for 

method modifications at 136.6.’’ Thus, 

an alternate sample container, 

preservation and/or holding time may 

be considered at the discretion of the 

permitting authority or other authority. 

2. Some stakeholders have asked EPA 

to extend the holding time for 

Escherichia coli and Enterococcus. In 

2006, EPA conducted a nationwide 

holding time study (EPA 2006) for fresh 

and marine ambient waters and 

concluded that, on a nationwide basis, 

the Agency was unable to justify 

extending the holding time for 

Escherichia coli or Enterococcus in 

these water matrices. However, EPA is 

proposing to provide some relief by 

revising footnote 22 to Table II, which 

applies to bacterial tests. This footnote 

currently reads as follows: ‘‘Sample 

analysis should begin immediately, 

preferably within 2 hours of collection. 

The maximum transport time to the 

laboratory is 6 hours, and samples 

should be processed (in incubator) 

within 2 hours of receipt at the 

laboratory.’’ 

Stakeholders have commented that 

laboratories must meet the two-hour 

analysis start time, even if they receive 

the samples early enough that they 

could start after two hours and still meet 

the overall six-hour time limit. EPA is 

proposing to revise the footnote 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.’’ 

3. EPA is proposing to revise 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. This 

practice advises analysts to add a 

reducing agent only if an oxidant is 

present, and use of the reducing agents 

sodium thiosulfate (Na2S2O3), ascorbic 

acid, sodium arsenite (NaAsO2), or 

sodium borohydride (NaBH4). 

4. EPA is proposing to revise 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. EPA proposes to allow 

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. 

5. EPA is proposing to revise footnote 

16 of Table II instructions for handling 

Whole Effluent Toxicity (WET) samples 

to be consistent with the November 19, 

2002 (67 FR 69951) ‘‘Guidelines for 

Establishing Test Procedures for the 

Analysis of Pollutants; Whole Effluent 

Toxicity Test Methods; Final Rule,’’ as 

well as the three toxicity methods 

(Methods for Measuring the Acute 

Toxicity of Effluents and Receiving 

Waters to Freshwater and Marine 

Organisms (5th Edition, October 2002), 

Short-term Methods for Estimating the 

Chronic Toxicity of Effluents and 

Receiving Waters to Freshwater 

Organisms (4th Edition, October 2002), 

and Short-term Methods for Estimating 

the Chronic Toxicity of Effluents and 

Receiving Waters to Marine and 

Estuarine Organisms (3rd Edition, 

October 2002). In the 2002 final rule, 

EPA established the acceptable range for 

the current sampling holding 

temperature for aquatic toxicity tests as 

0 to 6 °C based on current National 

Environmental Laboratory Accreditation 

Conference (NELAC) standards. EPA 

also clarified in the final rule that handdelivered samples used on the day of 

collection do not need to be cooled to 

0 to 6 °C prior to test initiation. Section 

8.5.1 of all three WET methods listed 

previously states, ‘‘Unless the samples 

are used in an on-site toxicity test the 

day of collection (or hand delivered to 

the testing laboratory for use on the day 

of collection) it is recommended that 

they be held at 0 to 6 °C until used to 

inhibit microbial degradation, chemical 

transformation, and loss of highly 

volatile toxic substances.’’ EPA is 

proposing to add two sentences to the 

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end of Footnote 16 of Table II based on 

this information. The two sentences are 

‘‘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 °C prior to test 

initiation.’’ 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.) 

6. EPA is proposing to add a sentence 

to footnote 4 of Table II to clarify the 

sample holding time for the Whole 

Effluent Toxicity (WET) samples for the 

three toxicity methods (Methods for 

Measuring the Acute Toxicity of 

Effluents and Receiving Waters to 

Freshwater and Marine Organisms (5th 

Edition, October 2002), Short-term 

Methods for Estimating the Chronic 

Toxicity of Effluents and Receiving 

Waters to Freshwater Organisms (4th 

Edition, October 2002), and Short-term 

Methods for Estimating the Chronic 

Toxicity of Effluents and Receiving 

Waters to Marine and Estuarine 

Organisms (3rd Edition, October 2002) 

to indicate that one sample of the 

minimum of three required samples 

may be used for the renewal of the test 

solutions and that the sample holding 

time refers to first use of each sample 

collected for the toxicity test. The 

sentence to be added is, ‘‘For staticrenewal 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 °C, with minimum head 

space.’’ 

G. Proposed Revisions to 40 CFR 136.4 

and 136.5 

EPA is proposing to revise §§ 136.4 

and 136.5 to describe the procedures for 

obtaining review and EPA approval for 

the use of alternate test procedures 

(alternate methods or ATPs). The 

proposed changes would revise 40 CFR 

136.4 to establish the procedures for 

obtaining approval for nationwide use 

of an ATP. The proposed changes would 

modify 40 CFR 136.5 to establish the 

procedures for obtaining approval for 

use of an ATP in a State within a 

particular EPA Region. It should be 

noted that in its ATP program, EPA 

considers for review only those methods 

for which EPA has published an ATP 

protocol. Presently, EPA has published 

protocols for chemistry, radiochemical, 

and culture microbiological methods. 

EPA does not have ATP protocols for 

Whole Effluent Toxicity (WET) methods 

or genetic methods. 

In today’s rule, EPA proposes to 

clarify that the intent of the limited use 

authority is to allow limited use of an 

alternate method for a specific 

application at a facility or type of 

discharge without requiring the same 

level of supporting test data that would 

be required for approval for nationwide 

use. Thus, limited use authority is not 

intended to be used as a means of 

avoiding the full examination of 

comparability that is required when 

EPA considers a method for nationwide 

use and decides to amend its list of 

approved CWA methods at 40 CFR part 

136 to include alternative test 

procedures. In the event that EPA 

decides not to approve an application 

for approval of an alternate method for 

nationwide use, the Regional Alternate 

Test Procedures Coordinator may 

choose to reconsider any previous 

limited use approvals of the alternate 

method. Based on this reconsideration, 

the Regional Coordinator will notify the 

user, if the limited use approval is 

withdrawn. 

H. Proposed Revisions to Method 

Modification Provisions at 40 CFR 136.6 

EPA encourages regulatory authorities 

to allow analysts the flexibility to 

modify CWA methods without prior 

approval provided the user has 

documented equivalent or better 

performance of the method in the matrix 

type to which the user will apply the 

modified method. EPA recognizes that 

addressing specific matrix interferences 

may require modifications to approved 

methods that do not require the 

extensive review and approval process 

specified for an alternate test procedure 

at 136.4 and 136.5. Based on users’ 

experiences with 136.6, since it was 

promulgated on March 12, 2007 (72 FR 

11199), EPA proposes to revise this 

section 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 

employed in methods currently 

approved in 40 CFR part 136. Analysts 

may use the examples in this section to 

assess and document that their 

modification is acceptable and does not 

depart substantially from the chemical 

principles in the method being 

modified. EPA specifically invites 

comment on the examples of flexibility 

specified at 136.6 and the 

documentation that a method modifier 

must have to demonstrate the 

equivalency of the modified method. In 

particular, EPA is interested in public 

comment on what additional controls, if 

any, should be applied when changing 

pH, purge times, buffers, or applying the 

relative standard error calibration 

alternative. 

I. Proposed New Quality Assurance and 

Quality Control Language at 40 CFR 

136.7 

EPA is proposing to specify 

‘‘essential’’ quality control at § 136.7 for 

use in conducting an analysis with an 

approved method and when insufficient 

instructions are contained in an 

approved method. Auditors, coregulators, laboratory personnel, and the 

regulated community have noted the 

different amounts and types of quality 

assurance (QA) and quality control (QC) 

procedures practiced by laboratories 

that use 40 CFR part 136 methods. Some 

of these methods are published by 

voluntary consensus standards bodies, 

such as the Standard Methods 

Committee, and ASTM International. 

ASTM and Standard Methods are 

contained in printed compendium 

volumes, electronic compendium 

volumes, or as individual online files. 

Each organization has its 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. For 

example, the publisher of Standard 

Methods for the Examination of Water 

and Wastewater consolidates the 

general quality assurance and quality 

control requirements for all methods. 

Each specific Part and section can 

contain additional QA and QC 

requirements (for example, see part 

2020, 3020, 6020, and 9020). ASTM 

specifies QA and QC requirements in 

the analyte method’s Referenced 

Documents section and in the analyte 

method. Both organizations require the 

analyst to reference this additional 

information within the respective 

compendiums to achieve the QA and 

QC expected for valid results. 

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 specific part 136 

method, or referenced these procedures 

by other means. Consequently, EPA 

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58036 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

expects that an analyst using these 

consensus body methods for reporting 

under the CWA will also comply with 

the quality assurance and quality 

control requirements listed in the 

appropriate sections in the consensus 

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 would 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 have insufficient 

QA/QC requirements, analysts could 

refer to and follow the QC published in 

several public sources. Examples of 

these sources include the instructions in 

an equivalent approved EPA method or 

standards published by the National 

Environmental Laboratory Accreditation 

Conference (cf. Chapter 5 of the 

compendium published in 2003.) 

In addition to and regardless of the 

source of the laboratory’s QA and QC 

instructions, EPA is proposing at 136.7 

to specify twelve essential quality 

control checks that must be in the 

laboratory’s documented quality system 

unless a written rationale is provided to 

explain why these controls are 

inappropriate for a specific analytical 

method or application. This written 

rationale will be included in the 

laboratory’s Standard Operating 

Procedure (SOP) for each method to 

which specific controls do not apply 

(e.g., internal standards, surrogate 

standards or tracers do not apply to 

analyses of inorganic parameters) as 

well as being included with the 

monitoring data produced using each 

method. 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. 

J. Proposed Withdrawal of Appendices 

at 40 CFR 136 

EPA is proposing to incorporate by 

reference all of the methods printed in 

40 CFR part 136 appendices A and C, 

and to remove most of the information 

in Appendix D. EPA is proposing to 

remove EPA Method numbers 601 

through 613, 624, 625, 1613B, 1624B 

and 1625B from Appendix A. All of 

these methods are readily accessible 

from a variety of sources including 

EPA’s CWA methods Web site http:// 

www.epa.gov/waterscience/methods/. 

Removing this appendix would decrease 

the resources associated with the annual 

publication of 40 CFR part 136 

regulations. EPA would incorporate 

these methods by reference in Tables IC 

and ID at 136.3(a). 

EPA is proposing to remove Appendix 

C—Method 200.7 Inductively Couple 

Plasma—Atomic Emission 

Spectrometric Method for Trace 

Element Analysis of Water and Waste 

Method because this method has been 

superseded by Rev. 5.4 of Method 200.7, 

which is incorporated by reference in 

Table IB. 

Finally, EPA is proposing to remove 

from Appendix D the data for all EPA 

methods that are no longer approved. 

This would result in Appendix D 

containing Precision and Recovery 

Statements only for EPA Method 279.2 

for thallium and EPA Method 289.2 for 

zinc. EPA will correct any typographical 

errors in the Appendix, such as the 

misspelling of thallium. EPA requests 

comment on whether to publish and 

make available, at least temporarily, the 

current version of Appendix D online at 

the CWA methods Web site for 

historical purposes. 

K. Proposed Revisions at 40 CFR 423 

EPA is proposing two changes to part 

423, Steam Electric Power Generating 

Point Source Category. First, EPA 

proposes to revise the definitions for 

total residual chlorine and free available 

chlorine at §§ 423.11(a) and 423.11(l), 

respectively. The current definitions 

restrict the permittee to the use of the 

specific amperometric titration method 

cited in the definitions. The revised 

definitions will allow the permittee 

flexibility to use additional approved 

methods. EPA proposes to revise the 

definitions as follows: 

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 

136.3(a), or other methods approved by 

the permitting authority. 

b. The term free available chlorine 

means the value obtained using any of 

the ‘‘chlorine—free available’’ methods 

in Table IB 136.3(a) where the method 

has the capability of measuring free 

available chlorine, or other methods 

approved by the permitting authority. 

Second, EPA is proposing to move the 

current citations of methods from Part 

423 and reference a new parameter, 

‘‘chlorine-free available’’, in Table IB at 

136.3(a). Under this parameter, EPA will 

list any Part 136 methods for total 

residual chlorine that also provide 

instructions for determining free 

chlorine. The tables at 136.3 are well 

known as the source of most methods 

that are approved for CWA programs. 

For this reason EPA is proposing to 

move the citations of specific methods 

from part 423 to Table IB, and as 

described in the following sections, also 

for Parts 430 and 435. 

L. Proposed Revisions at 40 CFR 430 

EPA is proposing several editorial 

changes to 40 CFR part 430, The Pulp, 

Paper, and Paperboard Point Source 

Category. Currently the complete text of 

EPA Methods 1650 and 1653 are 

published in Appendix A of part 430. 

EPA is proposing to cite these two 

methods in Table IC, at § 136.3, and to 

incorporate by reference the full text of 

these methods. EPA will list these two 

methods in Table IC—List of Approved 

Test Procedures for Non-Pesticide 

Organic Compounds, under adsorbable 

organic halides (AOX) by Method 1650 

and chlorinated phenolics by Method 

1653. This action would remove 

Appendix A at 40 CFR part 430, and 

organize the analytical methods for the 

Pulp, Paper, and Paperboard category 

into one part, the Part 136 CWA 

methods tables, of the CFR. 

To help users more readily identify 

approved compliance monitoring 

methods, EPA is proposing to cite at 

part 430 the Part 136 methods that are 

approved for these pollutants: 

Chloroform, 2,3,7,8- tetrachlorodibenzop-dioxin (TCDD), and 2,3,7,8- 

tetrachlorodibenzo-p-furan (TCDF). 

M. Proposed Revisions at 40 CFR 435 

EPA is proposing several changes to 

Part 435, Oil and Gas Extraction Point 

Source Category. EPA is proposing to 

move, and in two cases revise, the 

methods 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–09–013), which 

is included in the record for this 

rulemaking. This proposed 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 

proposes to move from Part 435 to the 

cited document, EPA–821–R–09–013. 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58037 

EPA METHOD NUMBERS FOR OIL AND GAS EXTRACTION POINT SOURCE CATEGORY ANALYTICAL METHODS AND PRIOR

CFR REFERENCES

Analytical/test method EPA method 

number 

Date first 

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 Sediments .................................................... 1646 2001 Subpart A, Appendix 3. 

Protocol for the Determination of Degradation of Non Aqueous Base Fluids in a 

Marine Closed Bottle Biodegradation Test System: Modified ISO 11734:1995.

1647 2001 Subpart A, Appendix 4. 

Determination of Crude Oil Contamination in Non-Aqueous Drilling Fluids by Gas 

Chromatography/Mass Spectrometry (GC/MS).

1655 2001 Subpart A, Appendix 5. 

Reverse Phase Extraction (RPE) Method for Detection of Oil Contamination in 

Non-Aqueous Drilling Fluids (NAF).

1670 2001 Subpart A, Appendix 6. 

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).

1674 2001 Subpart A, Appendix 7. 

EPA is also proposing to incorporate 

additional quality assurance procedures 

in the marine anaerobic biodegradation 

analytic method (Appendix 4 of Subpart 

A of Part 435) and to correct some 

erroneous references and omissions in 

the method for identification of crude 

oil contamination (Appendix 5 of 

Subpart A of Part 435). EPA is 

proposing to include these revisions in 

the EPA document (EPA–821–R–09– 

013). 

EPA promulgated the use of the 

marine anaerobic biodegradation 

analytic method (closed bottle test, ISO 

11734:1995 as clarified by Appendix 4 

to Subpart A of Part 435) 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 analytic 

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. 

Additionally, EPA is proposing to 

correct some erroneous references and 

omissions in the method for 

identification of crude oil 

contamination (Appendix 5 of Subpart 

A of Part 435). Specifically, EPA is 

proposing to: 

a. Add a schematic flow for 

qualitative identification of crude oil, 

which was erroneously omitted in 

Appendix 5 to Subpart A of Part 435, 

b. Correct erroneous citations in 

sections 9.5, 9.6, 11.3, and 11.3.1 of 

Appendix 5, and 

c. Add a missing ‘‘<’’ 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.’’ 

As previously noted, EPA is 

proposing to include these revisions to 

these two methods in the EPA 

document (EPA–821–R–09–013), which 

is included in the record for this 

rulemaking. 

III. Statutory and Executive Order 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and 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 the EO. 

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 updated 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 

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 proposed 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 

updated 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. 

In some cases, analytical costs may 

increase slightly due to the additional 

QC requirements included in the 

methods that are being approved to 

replace older EPA methods. However, 

most laboratories that analyze samples 

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58038 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

for EPA compliance monitoring have 

already instituted QC requirements as 

part of their laboratory practices. 

We continue to be interested in the 

potential impacts of the proposed rule 

on small entities and welcome 

comments on issues related to such 

impacts. 

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 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 updated versions of testing 

procedures. Thus, the proposed rule is 

not subject to the requirements of 

Section 203 of UMRA. 

E. Executive Order 13132: Federalism 

This proposed 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 proposed rule 

merely approves new and updated 

versions of testing procedures. The costs 

to State and local governments will be 

minimal (in fact, governments may see 

a cost savings), 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 solicits comment on this 

proposed action from State and local 

officials. 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

This proposed 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 

updated versions of testing procedures. 

The costs to Tribal governments will be 

minimal (in fact, governments may see 

a cost savings), and the rule does not 

preempt State law. 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 

solicits comment on this proposed 

action from tribal officials. 

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 

action proposes to approve new and 

updated versions of testing procedures. 

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 proposed rulemaking involves 

technical standards. As described 

throughout this document, EPA is 

proposing many standards developed by 

the Standard Methods Committee, and 

ASTM International. In Sections IIB, IIC 

of this preamble, and the tables at 

§ 136.3, EPA specifies these proposed 

methods, provides information on how 

to obtain copies of these methods, and 

describes the rationale for employing 

these methods. EPA welcomes 

comments on this aspect of the 

proposed rulemaking and, specifically, 

invites the public to identify potentially 

applicable voluntary consensus 

standards and to explain why EPA 

should include such standards in future 

revisions to Part 136. 

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 proposed 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 proposes to approve new and 

updated versions of testing procedures 

to measure pollutants in water. 

IV. References 

EPA 2006, ‘‘Assessment of the Effects of 

Holding Time on Enterococci 

Concentrations in Fresh and Marine 

Recreational Waters and Escherichia coli 

Concentrations in Fresh Recreational 

Waters’’ (EPA–821–R–06–019, December 

2006) 

EPA 2010a, ‘‘Method 1668A Interlaboratory 

Validation Study Report’’ (EPA–820–R– 

10–004, March 2010) 

EPA 2010b, ‘‘Addendum to the Method 

1668A Interlaboratory Validation Study 

Report’’ (EPA–820–R–10–003, March 

2010) 

EPA 2010c, ‘‘Peer Review of the Method 

1668A Interlaboratory Validation Study’’ 

(EPA 820–R–10–007, April 2010) 

EPA 2010d, ‘‘Development of Pooled Method 

Detection Limits (MDLs) and Minimum 

Levels of Quantitation (MLs) for EPA 

Method 1668C (May 2010) 

EPA 2010e, Errata for ‘‘Short-term Methods 

for Estimating the Chronic Toxicity of 

Effluents and Receiving Waters to 

Freshwater Organisms’’ (4th edition, 

October 2002) manual. 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58039 

OSS 2009, ASTM D7575 ‘‘Inter-Laboratory 

Study to Establish Precision Statements 

for ASTM WK23240—Standard Test 

Method for Solvent-Free Membrane 

Recoverable Oil and Grease by Infrared 

Determination’’ 

Passaic River 2010 ‘‘Summary of Passaic 

River Split Sample Results’’, EPA, April 

2010 

Test America 1 ‘‘Acrolein Acrylonitrile 

Stability Study’’ 

Test America 2 ‘‘Acrolein Acrylonitrile 

Control Charts’’ 

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: August 6, 2010. 

Lisa P. Jackson, 

Administrator. 

For the reasons set out in the 

preamble, title 40, chapter I of the Code 

of Federal Regulations, is proposed to be 

amended as follows: 

PART 136—GUIDELINES 

ESTABLISHING TEST PROCEDURES 

FOR THE ANALYSIS OF POLLUTANTS 

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.) 

2. Section 136.1 is amended by 

revising paragraph (a) to read as follows: 

§ 136.1 Applicability. 

(a) The procedures prescribed herein 

shall, except as noted in §§ 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. 

* * * * * 

3. Section 136.3 is amended: 

a. By revising paragraph (a) 

introductory text; 

b. In paragraph (a), revise Table IA, 

IB, IC, ID, IG, and IH; 

c. By revising paragraphs (b)(1), 

(b)(54), (b)(55), (b)(56), (b)(59), (b)(60), 

(b)(61), (b)(70), and adding paragraph 

(b)(73); 

d. By revising paragraph (e) 

introductory text; 

e. In Table II to paragraph (e), by 

revising entries ‘‘Table IA—Bacterial 

Tests’’, ‘‘Table IA—Aquatic Toxicity 

Tests’’, ‘‘Table IH—Bacterial Tests’’, and 

‘‘Table IH—Protozoan Tests, and 

footnote 6’’. 

These revisions and additions read as 

follows: 

§ 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. 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 

incorporation by reference of these 

documents, as specified in paragraph (b) 

of this section, was approved by 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 3334, 

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 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 § 136.4. 

Under certain circumstances paragraph 

(c) of this section, § 136.5 or 40 CFR 

401.13, other additional or alternate test 

procedures may be used. 

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 per 100 

mL or number 

per gram dry 

weight.

Most Probable Number 

(MPN), 5 tube, 3 dilution, or 

p. 132 3 .......................

1680 11, 13

1681 11, 18

9221 C E–2006.

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58040 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IA—LIST OF APPROVED BIOLOGICAL METHODS FOR WASTEWATER AND SEWAGE SLUDGE—Continued 

Parameter and units Method 1 EPA Standard methods AOAC, ASTM, 

USGS Other 

Membrane filter (MF) 2, 

single step.

p. 124 3 ....................... 9222 D–1997 .............. B–0050–85.4

2. Coliform (fecal) 

in presence of 

chlorine, number 

per 100 mL.

MPN, 5 tube, 3 dilution, or p. 132 3 ....................... 9221 C E–2006.

MF 2, single step ......... p. 124 3 ....................... 9222 D–1997.

3. Coliform (total), 

number per 100 

mL.

MPN, 5 tube, 3 dilution, or p. 114 3 ....................... 9221 B–2006.

MF 2, single step or 

two step.

p. 108 3 ....................... 9222 B–1997 .............. B–0025–85.4

4. Coliform (total), 

in presence of 

chlorine, number 

per 100 mL.

MPN, 5 tube, 3 dilution, or p. 114 3 ....................... 9221 B–2006.

MF 2 with enrichment .. p. 111 3 ....................... 9222 (B+B.5c)¥1997.

5. E. coli, number

per 100 mL.19

MPN 6, 8, 14 multiple 

tube/multiple well.

..................................... 9223 B–2004 12 ........... 991.15 10 ........... Colilert®12, 16

Colilert-18®.12 ,15, 16

MF 2, 5, 6, 7, 8 single 

step.

1603 20 ........................ ..................................... ........................... mColiBlue-24®.17

6. Fecal 

streptococci, 

number per 100 

mL.

MPN, 5 tube, 3 dilution, p. 139 3 ....................... 9230 B–2007.

MF 2, or ....................... p. 136 3 ....................... 9230 C–2007 .............. B–0055–85.4

Plate count .................. p. 143.3

7. Enterococci, 

number per 100.

mL.19

MPN 6 8, multiple tube/ 

multiple well.

..................................... ..................................... D6503–99 9 ....... Enterolert®.12 22

MF 25678 single step 1600.23

8. Salmonella, 

number per 

gram dry.

weight.11

MPN multiple tube ...... 1682.21

Aquatic Toxicity: 

9. Toxicity, acute, 

fresh water organisms, LC50, 

percent effluent.

Ceriodaphnia dubia 

acute.

2002.0.24

Daphnia puplex and 

Daphnia magna 

acute.

2021.0.24

Fathead minnow, 

Pimephales 

promelas, and 

Bannerfin shiner, 

Cyprinella leedsi, 

acute.

2000.0.24

Rainbow Trout, 

Oncorhynchus 

mykiss, and brook 

trout, Salvelinus 

fontinalis, acute.

2019.0.24

10. Toxicity, acute, 

estuarine and 

marine organisms of the Atlantic Ocean and 

Gulf of Mexico, 

LC50, percent effluent.

Mysid, Mysidopsis 

bahia, acute.

2007.0.24

Sheepshead Minnow, 

Cyprinodon 

variegatus, acute.

2004.0.24

Silverside, Menidia 

beryllina, Menidia 

menidia, and 

Menidia peninsulae, 

acute.

2006.0.24

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58041 

TABLE IA—LIST OF APPROVED BIOLOGICAL METHODS FOR WASTEWATER AND SEWAGE SLUDGE—Continued 

Parameter and units Method 1 EPA Standard methods AOAC, ASTM, 

USGS Other 

11. Toxicity, chronic, fresh water 

organisms, 

NOEC or IC25, 

percent effluent.

Fathead minnow, 

Pimephales 

promelas, larval survival and growth.

1000.0.25

Fathead minnow, 

Pimephales 

promelas, embryolarval survival and 

teratogenicity.

1001.0.25

Daphnia, Ceriodaphnia 

dubia, survival and 

reproduction.

1002.0.25

Green alga, 

Selenastrum 

capricornutum, 

growth.

1003.0.25

12. Toxicity, chronic, estuarine and 

marine organisms of the Atlantic Ocean and 

Gulf of Mexico, 

NOEC or IC25, 

percent effluent.

Sheepshead minnow, 

Cyprinodon 

variegatus, larval 

survival and growth.

1004.0.26

Sheepshead minnow, 

Cyprinodon 

variegatus, embryolarval survival and 

teratogenicity.

1005.0.26

Inland silverside, 

Menidia beryllina, 

larval survival and 

growth.

1006.0.26

Mysid, Mysidopsis 

bahia, survival, 

growth, and fecundity.

1007.0.26

Sea urchin, Arbacia 

punctulata, fertilization.

1008.0.26

1The method must be specified when results are reported. 

2A 0.45 μm 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 USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati, OH, EPA/600/8–78/017. 4 USGS. 1989. 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, U.S. Geological Survey, U.S. Department of the Interior, Reston, VA. 5Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be 

required to resolve any controversies. 6Tests 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. 7When 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. 8To 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. 9ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. ASTM International. 100 

Barr Harbor Drive, West Conshohocken, PA 19428. 10AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical 

Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877–2417. 11 Recommended for enumeration of target organism in sewage sludge. 12These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme b-glucuronidase produced by E. coli. 13 USEPA. April 2010. Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth 

(LTB) and EC Medium. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–10–003. 14Samples 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® may be enumerated with the multiple-well procedures, Quanti-Tray®, Quanti-Tray®/2000, and the MPN calculated from the table provided by the manufacturer. 15 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of 

incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples. 16 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc. 1 IDEXX 

Drive, Westbrook, ME 04092. 

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

58042 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

17A description of the mColiBlue24® test, is available from Hach Company. 100 Dayton Ave., Ames, IA 50010. 18 USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A–1 Medium. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–06–013. 19 Recommended for enumeration of target organism in wastewater effluent. 20 USEPA. December 2009. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant 

Escherichia coli Agar (modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–09–007. 21 USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. 

U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–06–014. 22A description of the Enterolert® test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092. 23 USEPA. December 2009. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b-D-Glucoside 

Agar (mEI). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–09–016. 24 USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. 

Fifth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R–02/012. 25 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. 

Fourth Edition, U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R–02/013. 26 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine 

Organisms. Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R–02/014. 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

1. Acidity, as CaCO3, 

mg/L.

Electrometric endpoint or 

phenolphthalein endpoint.

.................................. 2310 B–1997 ........... D1067–06 ................ I–1020–85.2

2. Alkalinity, as 

CaCO3, mg/L.

Electrometric or Colorimetric titration to pH 

4.5, Manual.

.................................. 2320 B–1997 ........... D1067–06 ................ 973.43,3 I–1030–85.2

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 36................................... 3111 D–1999 or E– 

1999.

.................................. I–3051–85.2

AA furnace .............. .................................. 3113–2004.

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

Direct Current Plasma (DCP) 36................................... .................................. D4190–08 ................ See footnote.34

Colorimetric 

(Eriochrome 

cyanine R).

.................................. 3500–Al B–2001.

4. Ammonia (as N), 

mg/L.

Manual distillation 6 or 

gas diffusion (pH > 11) 

followed by any of the 

following: 

350.1, Rev. 2.0 

(1993).

4500–NH3 B–1997 .. .................................. 973.49.3

Nesslerization .......... .................................. .................................. D1426–08 (A) .......... 973.49,3 I–3520–85.2

Titration ................... .................................. 4500–NH3 C–1997.

Electrode ................. .................................. 4500–NH3 D–1997 

or E–1997.

D1426–08 (B).

Manual phenate, salicylate, or other 

substituted phenols in Berthelot 

reaction based 

methods.

.................................. 4500–NH3 F–1997 ... .................................. See Footnote.60

Automated phenate, 

salicylate, or other 

substituted phenols in Berthelot 

reaction based 

methods.

350.1,30 Rev. 2.0 

(1993).

4500–NH3 G–1997 

4500–NH3 H–1997.

.................................. I–4523–85.2

Automated electrode .................................. .................................. .................................. See footnote 7. 

Ion Chromatography .................................. .................................. D6919–09.

5. Antimony—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration 36................................... 3111 B–1999.

AA furnace .............. .................................. 3113–2004.

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58043 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

6. Arsenic—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

206.5 (Issued 

1978).1

AA gaseous hydride .................................. 3114 B–2009 or C– 

2009.

D2972–08 (B) .......... I–3062–85.2

AA furnace .............. .................................. 3113–2004 ............... D2972–08 (C) .......... I–4063–98.49

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07.

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

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 aspiration 36................................... 3111 D–1999 ........... .................................. I–3084–85.2

AA furnace .............. .................................. 3113–2004 ............... D4382–02(07). 

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... .................................. I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

DCP36 ..................... .................................. .................................. .................................. See footnote.34

8. Beryllium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 D–1999 or E– 

1999.

D3645–08 (A) .......... I–3095–85.2

AA furnace .............. .................................. 3113–2004 ............... D3645–08 (B).

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

DCP ......................... .................................. .................................. D4190–08 ................ See footnote.34

Colorimetric 

(aluminon).

.................................. .................................. .................................. See footnote.61

9. Biochemical oxygen 

demand (BOD5), 

mg/L.

Dissolved Oxygen Depletion................................... 5210 B–2001 ........... D888–09 .................. 973.44,3 p. 17,9 I– 

1578–78,8 See 

footnote.10 63

10. Boron—Total,37

mg/L.

Colorimetric (curcumin) .. .................................. 4500–B B–2000 ....... .................................. I–3112–85.2

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000, C– 

2000, D–2000.

D4327–03 ................ 993.30.3

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

12. Cadmium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration 36................................... 3111 B–1999 or C– 

1999.

D3557–02(07) (A or 

B).

974.27,3 p. 37.9, 

I–3135–85 2 or 

I–3136–85.2

AA furnace .............. .................................. 3113–1999 ............... D3557–02(07) (D) .... I–4138–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–1472–85 2 or 

I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

Voltametry 11 ........... .................................. .................................. D3557–02(07)(C).

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58044 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Colorimetric (Dithizone) .................................. 3500 Cd–D 1990.

13. Calcium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999 ........... D511–08(B) ............. I–3152–85.2

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... .................................. I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

DCP ......................... .................................. .................................. .................................. See footnote.34

Titrimetric (EDTA) ... .................................. 3500–Ca–1997 ........ D511–08(A).

Ion Chromatography .................................. .................................. D6919–09.

14. Carbonaceous biochemical oxygen demand (CBOD5), mg/ 

L.12

Dissolved Oxygen Depletion with nitrification inhibitor................................... 5210 B–2001 ........... D888–09 .................. See footnote.35 63

15. Chemical oxygen 

demand (COD), mg/ 

L.

Titrimetric ........................ 410.3 (Rev. 1978) 1 5220 B–1997 or C– 

1997.

D1252–06 (A) .......... 973.46,3 p. 17 9

I–3560–85.2

Spectrophotometric, 

manual or automatic.

410.4, Rev. 2.0 

(1993).

5220 D–1997 ........... D1252–06 (B) .......... See footnotes.13 14

I–3561–85.2

16. Chloride, mg/L ...... Titrimetric: (silver nitrate) .................................. 4500–Cl¥ B–1997 ... D512–04 (B) ............ I–1183–85.2

(Mercuric nitrate) ............ .................................. 4500–Cl¥ C–1997 ... D512–04 (A) ............ 973.51,3 I–1184–85.2

Colorimetric: manual ...... .................................. .................................. .................................. I–1187–85.2

Automated (Ferricyanide) .................................. 4500–Cl¥ E–1997 ... .................................. I–2187–85.2

Potentiometric Titration .. .................................. 4500–Cl¥ D–1997.

Ion Selective Electrode .. .................................. .................................. D512–04 (C).

Ion Chromatography ....... 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30,3 I–2057– 

90.51

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

17. Chlorine—Total residual, mg/L.Amperometric direct ....... .................................. 4500–Cl D–2000 ..... D1253–08.

Amperometric direct (low 

level).

.................................. 4500–Cl E–2000.

Iodometric direct ............. .................................. 4500–Cl B–2000.

Back titration ether end– 

point 15.

.................................. 4500–Cl C–2000.

DPD–FAS ....................... .................................. 4500–Cl F–2000.

Spectrophotometric, DPD .................................. 4500–Cl G–2000.

Electrode ........................ .................................. .................................. .................................. See footnote.16

17A. Chlorine—Free 

Available, mg/L.

Amperometric direct ....... .................................. 4500–Cl D–2000 ..... D1253–08.

Amperometric direct (low 

level).

.................................. 4500–Cl E–2000.

DPD–FAS ....................... .................................. 4500–Cl F–2000.

Spectrophotometric, DPD .................................. 4500–Cl G–2000.

18. Chromium VI dissolved, mg/L.0.45-micron Filtration followed by any of the 

following: 

AA chelation-extraction................................... 3111 C–1999 ........... .................................. I–1232–85.2

Ion Chromatography 218.6, Rev. 3.3 

(1994).

3500–Cr C–2009 ..... D5257–03 ................ 993.23. 

Colorimetric (Diphenyl-carbazide)................................... 3500–Cr B–2009 ..... D1687–02(07)(A) ..... I–1230–85.2

19. Chromium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration 36................................... 3111 B–1999 ........... D1687–02(07) (B) .... 974.27,3 I–3236–85.2

AA chelation-extraction................................... 3111 C–1999.

AA furnace .............. .................................. 3113–1999 ............... D1687–02(07)(C) ..... I–3233–93.46

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58045 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Colorimetric (Diphenyl-carbazide)................................... 3500–Cr B–2009.

20. Cobalt—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999 or C– 

1999.

D3558–08 (A or B) .. p. 37,9 I–3239–85.2

AA furnace .............. .................................. 3113–2004 ............... D3558–08 (C) .......... I–4243–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES .................. 200.7, Rev. 4.4 

(1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

DCP ......................... .................................. .................................. D4190–08 ................ See footnote.34

21. Color, platinum cobalt units or dominant wavelength, 

hue, luminance purity.

Colorimetric (ADMI) ........ .................................. .................................. .................................. See footnote.18

(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 aspiration.36.................................. 3111 B–1999 or C– 

1999.

D1688–07 (A or B) .. 974.27 3 p. 37 9

I–3270–85 2 or 

I–3271–85.2

AA furnace .............. .................................. 3113–2004 ............... D1688–07 (C) .......... I–4274–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05 

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

Colorimetric 

(Neocuproine).

.................................. 3500–Cu B–1999.

(Bathocuproine) ....... .................................. 3500–Cu C–1999 .... .................................. See footnote.19

23. Cyanide—Total, 

mg/L.

Automated UV digestion/ 

distillation and Colorimetry.

.................................. .................................. .................................. Kelada–01.55

Segmented Flow Injection, In-Line Ultraviolet 

Digestion followed by 

gas diffusion amperometry.

.................................. .................................. D7511–09e2.

Manual distillation with 

MgCl2 followed by any 

of the following: 

335.4, Rev. 1.0 

(1993) 57.

4500–CN¥ B–1999 

or C–1999.

D2036–09(A), 

D7284–08.

10–204–00–1–X.56

Flow Injection, gas 

diffusion amperometry.

.................................. .................................. D2036–09(A) 

D7284–08.

Titrimetric ................. .................................. 4500–CN¥ D–1999 D2036–09(A) ........... p. 22.9

Spectrophotometric, 

manual.

.................................. 4500–CN¥ E–1999 D2036–09(A) ........... I–3300–85.2

Semi-Automated 20 .. 335.4, Rev. 1.0 

(1993) 57.

.................................. .................................. 10–204–00–1–X,56

I–4302–85.2

Ion Chromatography .................................. .................................. D2036–09(A).

Ion Selective Electrode................................... 4500–CN¥ F–1999 D2036–09(A).

24. Cyanide-Available, 

mg/L.

Cyanide Amenable to 

Chlorination (CATC); 

Manual distillation with 

MgCl2 followed by 

Titrimetric or 

Spectrophotometric.

.................................. 4500–CN¥ G–1999 D2036–09(B).

Flow injection and ligand 

exchange, followed by 

gas diffusion amperometry 59.

.................................. .................................. D6888–09 ................ OIA–1677–09.44

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58046 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Automated Distillation 

and Colorimetry (no 

UV digestion).

.................................. .................................. .................................. Kelada–01.55

24.A Cyanide-Free, 

mg/L.

Flow Injection, followed 

by gas diffusion amperometry.

.................................. .................................. D7237–10 ................ OIA–1677–09.44

Manual micro-diffusion 

and colorimetry.

.................................. .................................. D4282–02.

25. Fluoride—Total, 

mg/L.

Manual distillation 6 followed by any of the 

following: 

.................................. 4500–F¥ B–1997.

Electrode, manual ... .................................. 4500–F¥ C–1997 .... D1179–04(B).

Electrode, automated................................... .................................. .................................. I–4327–85.2

Colorimetric, 

(SPADNS).

.................................. 4500–F¥ D–1997 .... D1179–04(A).

Automated 

complexone.

.................................. 4500–F¥ E–1997.

Ion Chromatography 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30.3

CIE/UV .................... .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

26. Gold—Total,4 mg/ 

L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration, .................................. 3111 B–1999.

AA furnace, ............. 231.2 (Rev. 1978) 1 3113–2004.

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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) .......... 973.5 2B,3 I–1338– 

85.2

Ca plus Mg as their carbonates, by inductively 

coupled plasma or AA 

direct aspiration. (See 

Parameters 13 and 33).

.................................. 2340 B–1997.

28. Hydrogen ion (pH), 

pH units.

Electrometric measurement................................... 4500–H+–2000 ........ D1293–99 (A or B) .. 973.41,3 I–1586–85.2

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 aspiration .................................. 3111 B–1999.

AA furnace .............. 235.2 (Issued 

1978).1

ICP/MS .................... .................................. 3125–2009.

30. Iron—Total,4 mg/L Digestion 4 followed by 

any of the following: 

AA direct aspiration 36................................... 3111 B–1999 or C– 

1999.

D1068–05 (A or B) .. 974.27,3 I–3381–85.2

AA furnace .............. .................................. 3113–1999 ............... D1068–05(C).

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

Colorimetric (Phenanthroline)................................... 3500–Fe-1997 ......... D1068–05 (D) .......... See footnote.22

31. Kjeldahl Nitrogen 5—Total, (as N), 

mg/L.

Manual digestion 20 and 

distillation or gas diffusion followed by any of 

the following: 

.................................. 4500–Norg B–1997 

or C–1997 and 

4500–NH3 B–1997.

D3590–02(06)(A) ..... I–4515–91.45

Titration ................... .................................. 4500–NH3 C–1997 .. .................................. 973.48.3

Nesslerization .......... .................................. .................................. D1426–08(A).

Electrode ................. .................................. 4500–NH3 D–1997 

or E–1997.

D1426–08(B).

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58047 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Semi-automated 

phenate.

350.1 Rev. 2.0 1993 4500–NH3 G–1997 

4500–NH3 H–1997.

Manual phenate, salicylate, or other 

substituted phenols in Berthelot 

reaction based 

methods.

.................................. 4500–NH3 F–1997 ... .................................. See Footnote.60

Automated Methods for TKN that do not require manual distillation 

Automated phenate, salicylate, or other substituted phenols in 

Berthelot reaction 

based methods colorimetric (auto digestion 

and distillation).

351.1, (Rev. 1978) 1 .................................. .................................. I–4551–78.8

Semi-automated block 

digestor colorimetric 

(distillation not required).

351.2, Rev. 2.0 

(1993).

4500–Norg D–1997 D3590–02(06) (B) .... I–4515–91.45

Block digester, followed 

by Auto distillation and 

Titration.

.................................. .................................. .................................. See footnote.39

Block digester, followed 

by Auto distillation and 

Nesslerization. 

.................................. .................................. .................................. See footnote.40

Block Digester, followed 

by Flow injection gas 

diffusion (distillation 

not required).

.................................. .................................. .................................. See footnote.41

32. Lead—Total,4 mg/ 

L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration.36.................................. 3111 B–1999 or C– 

1999.

D3559–08(A or B) ... 974.27,3 I–3399–85.2

AA furnace .............. .................................. 3113–1999 ............... D3559–08(D) ........... I–4403–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

Voltametry 11 ........... .................................. .................................. D3559–08(C).

Colorimetric (Dithizone)................................... 3500–Pb B–1997.

33. Magnesium— 

Total,4 mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999 ........... D511–08(B) ............. 974.27,3 I–3447–85.2

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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: 

AA direct aspiration 36................................... 3111 B–1999 ........... D858–07(A or B) ..... 974.27,3 I–3454–85.2

AA furnace .............. .................................. 3113–2004 ............... D858–07(C).

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4471– 

97.50

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

58048 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Colorimetric 

(Persulfate).

.................................. 3500–Mn B–1999 .... .................................. 920.203.3

(Periodate) ............... .................................. .................................. .................................. See footnote.23

35. Mercury—Total,4

mg/L.

Cold vapor, Manual ........ 245.1, Rev. 3.0 

(1994).

3112–2009 ............... D3223–07 ................ 977.22,3 I–3462–85.2

Cold vapor, Automated .. 245.2 (Issued 1974).

Cold vapor atomic fluorescence spectrometry 

(CVAFS).

245.7, Rev. 2.0 

(2005) 17.

.................................. .................................. I–4464–01. 

Purge and Trap CVAFS 1631E.43

ICP/AES36 ...................... 200.7, Rev. 4.4 

(1994).

3120–1999 ............... .................................. I–4471–97.50

ICP/MS ........................... .................................. 3125–2009.

36. Molybdenum— 

Total,4 mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 D–1999 ........... .................................. I–3490–85.2

AA furnace .............. .................................. 3113–2004 ............... .................................. I–3492–96.47

ICP/AES .................. 200.7, Rev. 4.4 

(1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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 aspiration 36................................... 3111 B–1999 or C– 

1999.

D1886–08(A or B) ... I–3499–85.2

AA furnace .............. .................................. 3113–2004 ............... D1886–08(C) ........... I–4503–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

38. Nitrate (as N), mg/ 

L.

Ion Chromatography ....... 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30.3

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

Ion Selective Electrode .. .................................. 4500–NO3

¥ D–2000.

Colorimetric (Brucine sulfate).352.1 1 ...................... .................................. .................................. 973.50,3 419D,1 7 p. 

28.9

Nitrate-nitrite N minus Nitrite N (See parameters 39 and 40)................................... .................................. .................................. See footnote.62

39. Nitrate-nitrite (as 

N), mg/L.

Cadmium reduction, 

Manual.

.................................. 4500–NO3

¥ E–2000 D3867–04(B).

Cadmium reduction, 

Automated.

353.2, Rev. 2.0 

(1993).

4500–NO3

¥ F–2000 D3867–04(A) ........... I–2545–90.2

Automated hydrazine ..... .................................. 4500–NO3

¥ H–2000.

Reduction/Colorimetric ... .................................. .................................. .................................. See footnote.62

Ion Chromatography ....... 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30.3

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

40. Nitrite (as N), mg/L Spectrophotometric: 

Manual.

.................................. 4500–NO2

¥ B–2000 .................................. See footnote.25

Automated 

(Diazotization).

.................................. .................................. .................................. I–4540–85,2 See 

footnote.62

Automated (*bypass cadmium reduction).353.2, Rev. 2.0 

(1993).

4500–NO3

¥ F–2000 D3867–04 (A) .......... I–4545–85.2

Manual (*bypass cadmium reduction)................................... 4500–NO3

¥ E–2000 D3867–04 (B).

Ion Chromatography ....... 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30.3

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev.2.54

41. Oil and grease— 

Total recoverable, 

mg/L.

Hexane extractable material (HEM): n-Hexane 

extraction and gravimetry.

1664B42 ................... 5520 B–2001.38

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58049 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Silica gel treated HEM 

(SGT–HEM): Silica gel 

treatment and gravimetry. 

1664B42 ................... 5520 B–2001 38 and 

5520 F–2001.38

42. Organic carbon— 

Total (TOC), mg/L.

Combustion .................... .................................. 5310 B–2000 ........... D7573–09 ................ 973.47,3 p. 14.24

Heated persulfate or UV 

persulfate oxidation.

.................................. 5310 C 2000 5310 D 

2000.

D4839–03 ................ 973.47,3 p. 14.24

43. Organic nitrogen 

(as N), mg/L.

Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4).

44. Orthophosphate 

(as P), mg/L.

Ascorbic acid method: 

Automated ............... 365.1, Rev. 2.0 

(1993).

4500–P F–1999 or 

G–1999.

.................................. 973.56,3 I–4601–85.2

Manual single reagent................................... 4500–P E–1999 ....... D515–88(A) ............. 973.55.3

Manual two reagent 365.3 (Issued 

1978).1

Ion Chromatography 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30.3

CIE/UV .................... .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

45. Osmium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 D–1999.

AA furnace .............. 252.2 (Issued 

1978) 1

46. Oxygen, dissolved, 

mg/L.

Winkler (Azide modification)................................... 4500–O B–2001, C– 

2001, D–2001, E– 

2001, F–2001.

D888–09(A) ............. 973.45B,3 I–1575– 

78.8

Electrode ........................ .................................. 4500–O G–2001 ...... D888–09(B) ............. I–1576–78.8

Luminescence Based 

Sensor.

.................................. .................................. D888–09 68 (C) ........ See footnote 63 68

See footnote.64

47. Palladium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999.

AA furnace .............. 253.2 1 (Issued 

1978).

ICP/MS .................... .................................. 3125–2009.

DCP ......................... .................................. .................................. .................................. See footnote.34

48. Phenols, mg/L ...... Manual distillation 26 followed by any of the 

following: 

420.1 1 (Rev. 1978) 5530B–2005 ............ D1783–01.

Colorimetric (4AAP) 

manual.

420.1 1 (Rev. 1978) 5530D–2005 27 ........ D1783–01(A or B).

Automated colorimetric (4AAP).420.4, Rev. 1.0 

(1993).

49. Phosphorus (elemental), mg/L.Gas–liquid chromatography................................... .................................. .................................. See footnote.28

50. Phosphorus— 

Total, mg/L.

Persulfate digestion 20

followed by any of the 

following: 

.................................. 4500–P B(5)–1999 .. .................................. 973.55.3

Manual ..................... 365.3 1 (Issued 

1978).

4500–P E–1999 ....... D515–88(A).

Automated ascorbic 

acid reduction.

365.1, Rev. 2.0 

(1993).

4500–P F–1999, G– 

1999, H–1999.

.................................. 973.56,3 I–4600–85.2

ICP/AES4 36 ............ 200.7, Rev. 4.4 

(1994).

3120–1999 ............... .................................. I–4471–97.50

Semi–automated 

block digestor 

(TKP digestion).

365.4 1 (Issued 

1974).

.................................. D515–88(B) ............. I–4610–91.48

51. Platinum—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999.

AA furnace .............. 255.2.1

ICP/MS .................... .................................. 3125–2009.

DCP ......................... .................................. .................................. .................................. See footnote.34

52. Potassium— 

Total,4 mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999 ........... .................................. 973.53,3 I–3630–85.2

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58050 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

ICP/AES .................. 200.7, Rev. 4.4 

(1994).

3120–1999.

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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, 103–105° .... .................................. 2540 B–1997 ........... .................................. I–3750–85.2

54. Residue—filterable, mg/L.Gravimetric, 180° ........... .................................. 2540 C–1997 ........... D5907–03 ................ I–1750–85.2

55. Residue—non–filterable (TSS), mg/L.Gravimetric, 103–105° 

post washing of residue.

.................................. 2540 D–1997 ........... D5907–03 ................ I–3765–85.2

56. Residue—settleable, mg/L.Volumetric, (Imhoff 

cone), or gravimetric.

.................................. 2540 F–1997.

57. Residue—Volatile, 

mg/L.

Gravimetric, 550° ........... 160.4 1 ...................... 2540–E–1997 .......... .................................. I–3753–85.2

58. Rhodium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration, 

or.

.................................. 3111 B–1999.

AA furnace .............. 265.2.1

ICP/MS .................... .................................. 3125–2009.

59. Ruthenium— 

Total,4 mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration, 

or.

.................................. 3111 B–1999.

AA furnace .............. 267.2.1

ICP/MS .................... .................................. 3125–2009.

60. Selenium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA furnace .............. .................................. 3113–2004 ............... D3859–08 (B) .......... I–4668–98.49

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07.

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05 

AA gaseous hydride .................................. 3114 B–2009, or C– 

2009.

D3859–08 (A) .......... I–3667–85.2

61. Silica—Dissolved,37 mg/L.0.45 micron filtration followed by any of the 

following: 

Colorimetric, Manual .................................. 4500–SiO2 C–1997 D859–05 .................. I–1700–85.2

Automated 

(Molybdosilicate).

.................................. 4500–SiO2 E–1997 

or F–1997.

.................................. I–2700–85.2

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... .................................. I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

62. Silver—Total,4 31

mg/L.

Digestion 4 29 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999 or C– 

1999.

.................................. 974.27,3 p. 37,9 I– 

3720–85.2

AA furnace .............. .................................. 3113 –1999 ............. .................................. I–4724–89.51

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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 aspiration .................................. 3111 B–1999 ........... .................................. 973.54,3 I–3735–85.2

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... .................................. I–4471–97.50

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58051 

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

DCP ......................... .................................. .................................. .................................. See footnote.34

Flame photometric .. .................................. 3500–Na B–1997.

Ion Chromatography .................................. .................................. D6919–09.

64. Specific conductance, micromhos/cm 

at 25 °C.

Wheatstone bridge ......... 120.1 1 (Rev. 1982) 2510 –1997 ............. D1125–99 (A) .......... 973.40,3 I–2781–85.2

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 or D–1997.

.................................. 925.54.3

Turbidimetric ................... .................................. 4500–SO4

2¥ E– 

1997.

D516–07.

Ion Chromatography ....... 300.0, Rev. 2.1 

(1993) and 300.1, 

Rev. 1.0 (1997).

4110 B–2000 or C– 

2000.

D4327–03 ................ 993.30,3 I–4020–05. 

CIE/UV ............................ .................................. 4140–1997 ............... D6508–00(05) .......... D6508, Rev. 2.54

66. Sulfide (as S), mg/ 

L.

Sample Pretreatment ..... .................................. 4500–S2¥ B, C– 

2000.

Titrimetric (iodine) ........... .................................. 4500–S2¥ F–2000 .. .................................. I–3840–85.2

Colorimetric (methylene 

blue).

.................................. 4500–S2¥ D–2000.

Ion Selective Electrode .. .................................. 4500–S2¥ G–2000 D4658–08.

67. Sulfite (as SO3), 

mg/L.

Titrimetric (iodine-iodate) .................................. 4500–SO3

2¥ B– 

2000.

68. Surfactants, mg/L Colorimetric (methylene 

blue).

.................................. 5540 C–2000 ........... D2330–02.

69. Temperature, °C .. Thermometric ................. .................................. 2550 B–2000 ........... .................................. See footnote.32

70. Thallium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 B–1999.

AA furnace .............. 279.2 1 (Issued 

1978).

3113–2004.

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES .................. 200.7, Rev. 4.4 

(1994).

3120–1999 ............... D1976–07.

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... 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 aspiration .................................. 3111 B–1999 ........... .................................. I–3850–78.8

AA furnace .............. .................................. 3113–2004.

STGFAA .................. 200.9, Rev. 2.2 

(1994).

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

72. Titanium—Total,4

mg/L.

Digestion 4 followed by 

any of the following: 

AA direct aspiration .................................. 3111 D–1999.

AA furnace .............. 283.2 1(Issued 1978).

DCP ......................... .................................. .................................. .................................. See footnote.34

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14.3

73. Turbidity, NTU 53 .. Nephelometric ................ 180.1, Rev. 2.0 

(1993).

2130–2001 ............... 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 aspiration .................................. 3111 D–1999.

AA furnace .............. .................................. 3113–2004 ............... D3373–03(07).

ICP/AES .................. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

DCP ......................... .................................. .................................. D4190–08 ................ See footnote.34

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TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued 

Parameter Methodology 58 EPA52 Standard methods ASTM USGS/AOAC/other 

Colorimetric (Gallic 

Acid).

.................................. 3500–V B–1997.

75. Zinc—Total,4 mg/L Digestion 4 followed by 

any of the following: 

AA direct aspiration 36................................... 3111 B–1999 or C– 

1999.

D1691–02(07) (A or 

B).

974.27,3 p. 37,9

I–3900–85.2

AA furnace .............. 289.21 (Issued 1978).

ICP/AES36 .............. 200.5, Rev. 4.2 

(2003); 200.7, 

Rev. 4.4 (1994).

3120–1999 ............... D1976–07 ................ I–4471–97.50

ICP/MS .................... 200.8, Rev. 5.4 

(1994).

3125–2009 ............... D5673–05 ................ 993.14,3 I–4020–05. 

DCP36 ..................... .................................. .................................. D4190–08 ................ See footnote.34

Colorimetric (Dithizone).

(Zincon) ................... .................................. 3500–Zn–1997 ........ .................................. See footnote.33

76. Acid Mine Drainage.......................................... 1627.

Table 1B Notes: 

1 ‘‘Methods for Chemical Analysis of Water and Wastes,’’ Environmental Protection Agency, Environmental Monitoring Systems Laboratory— 

Cincinnati (EMSL–CI), EPA–600/4–79–020 (NTIS PB 84–128677), Revised March 1983 and 1979 where applicable. 2Fishman, M. J., et al. ‘‘Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,’’ U.S. Department of the Interior, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated. 3 ‘‘Official Methods of Analysis of the Association of Official Analytical Chemists,’’ Methods Manual, Sixteenth Edition, 4th Revision, 1998. 4For 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. 7Ammonia, Automated Electrode Method, Industrial Method Number 379–75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto 

Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523. 8The approved method is that cited in ‘‘Methods for Determination of Inorganic Substances in Water and Fluvial Sediments’’, USGS TWRI, 

Book 5, Chapter A1 (1979). 9American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd St., New York, NY 

10036. 10 In-Situ Method 1003–8–2009, ‘‘Biochemical Oxygen Demand (BOD) Measurement by Optical Probe’’. Available from In-Situ, Incorporated, 

221 E. Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970–498–1500. 11The 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. 13OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 151 Graham Road, P.O. Box 9010, College Station, 

TX 77842. 14 Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 

80537. 15The back titration method will be used to resolve controversy. 16Orion Research Instruction Manual, Residual Chlorine Electrode Model 97–70, 1977, Orion Research Incorporated, 840 Memorial Drive, 

Cambridge, MA 02138. 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, Rev. 2.0, ‘‘Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,’’ February 2005, EPA–821–R–05–001, available from the U.S. EPA Sample Control Center (operated by CSC), 6101 Stevenson Avenue, Alexandria, VA 22304, Telephone: 703–461–2100, 

Fax: 703–461–8056. 18 National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971. 19 Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, 

CO 80537. 20When using a method with block digestion, this treatment is not required. 21 Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378–75WA, October 1976, Bran & Luebbe (Technicon) 

Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523. 

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22 Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 23 Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2–113 and 2–117, Hach 

Chemical Company, Loveland, CO 80537. 24Wershaw, R. L., et al., ‘‘Methods for Analysis of Organic Substances in Water,’’ Techniques of Water-Resources Investigation of the U.S. 

Geological Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14. 25 Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 26 Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH. 27The colorimetric reaction must be conducted at a pH of 10.0 ± 0.2. 28 R.F. Addison and R. G. Ackman, ‘‘Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,’’ Journal of Chromatography, Vol. 47, No. 3, pp. 421–426, 1970. 29Approved 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. 30The 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. 31For 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. 32Stevens, H. H., Ficke, J. F., and Smoot, G. F., ‘‘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. 33Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2–231 and 2–333, Hach Chemical Company, Loveland, 

CO 80537. 34 ‘‘Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method 

AES0029,’’ 1986—Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge Parkway, Franklin, MA 02038. 35 In-Situ Method 1004–8–2009, ‘‘Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe’’. Available from In-Situ, 

Incorporated, 221 E. Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970–498–1500. 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’’, CEM Corporation, P.O. Box 200, Matthews, NC 28106–0200, April 16, 1992. Available from 

the CEM Corporation. 37When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. 38Only 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 Method 1664B). 

Use of other extraction solvents is prohibited. 39 Nitrogen, Total Kjeldahl, Method PAI–DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ 

ALPKEM, P.O. Box 9010, College Station, TX 77842. 40 Nitrogen, Total Kjeldahl, Method PAI–DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ 

ALPKEM, P.O. Box 9010, College Station, TX 77842. 41 Nitrogen, Total Kjeldahl, Method PAI–DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/96, OI Analytical/ALPKEM, P.O. 

Box 9010, College Station, TX 77842. 42 Method 1664, Revision B is the revised version of EPA Method 1664A. 43 USEPA. 2001. Method 1631, Revision E, ‘‘Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry’’ September 2002, Office of Water, U.S. Environmental Protection Agency (EPA–821–R–02–024). The application of clean techniques described in EPA’s draft 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. 44Available Cyanide, Method OIA–1677–09, ‘‘Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,’’ ALPKEM, A Division 

of OI Analytical, P.O. Box 9010, College Station, TX 77842–9010. 45 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonia Plus Organic Nitrogen 

by a Kjeldahl Digestion Method,’’ Open File Report (OFR) 00–170. 46 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite 

Furnace Atomic Absorption Spectrophotometry,’’ Open File Report (OFR) 93–449. 47 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace 

Atomic Absorption Spectrophotometry,’’ Open File Report (OFR) 97–198. 48 ‘‘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’’ Open File Report (OFR) 92–146. 49 ‘‘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’’ Open File Report (OFR) 98–639. 50 ‘‘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,’’ Open File Report (OFR) 

98–165. 51 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment,’’ Open File Report (OFR) 93–125. 52 Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, are published in ‘‘Methods for the Determination of Metals in 

Environmental Samples,’’ Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL–CI), EPA/600/R–94/111, May 1994; and ‘‘Methods 

for the Determination of Inorganic Substances in Environmental Samples,’’ NERL–CI, EPA/600/R–93/100, August, 1993. EPA Method 300.1 is 

available from http://www.epa.gov/safewater/methods/pdfs/met300.pdf. 53Styrene divinyl benzene beads (e.g., AMCO–AEPA–1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin. 54 Method D6508, Rev. 2, ‘‘Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,’’ available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482–2131, Fax: 508/482– 

3625. 55Kelada-01, ‘‘Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,’’ EPA 821–B–01–009, Revision 

1.2, August 2001, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 [Order Number PB 2001– 

108275]. 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. 56QuikChem 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’’ is available from Lachat Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414– 

358–4200. 

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57When using sulfide removal test procedures described in Method 335.4, 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. 59Samples analyzed for available cyanide using Methods OIA–1677–09 or 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. 60Analysts 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, C.J. 

Patton and S.R. Crouch, Anal. Chem. (1977) 49, 464–469. These reaction parameters increase to pH >12.6 and 665 nm when salicylate is used 

as the color reagent—see, M.D. Krom, Analyst (1980) 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. 62Systea Easy (1-Reagent) Nitrate Method, February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific, LLC., 900 Jorie 

Blvd., Suite 35, Oak Brook, IL 60523. 63 Hach Method 10360, ‘‘Luminescence Measurement of Dissolved Oxygen (LDO®) in Water and Wastewater, Revision 1.1 dated January 4, 

2006’’. Available from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539, Telephone: 970–669–3050. 64 In-Situ Method 1002–8–2009, ‘‘Dissolved Oxygen (DO) Measurement by Optical Probe’’, 1003–8–2009. Available from In-Situ, Incorporated, 

221 E. Lincoln Avenue, Ft. Collins, CO 80524, Telephone: 970–498–1500. 65 Mitchell Method M5331, ‘‘Determination of Turbidity by Nephlometry’’, Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 

656 Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630–645–0600. 66 Mitchell Method M5271, ‘‘Determination of Turbidity by Nephlometry’’, Revision 1.0, July 31, 2008. Available from Leck Mitchell, Ph.D., P.E., 

656 Independence Valley Drive, Grand Junction Colorado 81507, Phone: 630–645–0600. 67Thermo Scientific’s Orion Method AQ4500, Revision 5, March 12, 2009, ‘‘Determination of Turbidity by Nephlometry’’. Available from Thermo 

Scientific, 166 Cummings Center, Beverly, MA 01915, Phone: 1–800–225–1480, http://www.thermo.com. 68This method may be used to measure dissolved oxygen when performing methods approved in Table 1B for measurement of biochemical

oxygen demand for compliance monitoring under the Clean Water Act. 

TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

1. Acenaphthene .................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

2. Acenaphthylene ................................................. GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

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–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440B–00 ......... D4657–92 (99).

6. Benzene ............................................................. GC .................... 602 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

7. Benzidine ........................................................... Spectrophotometric............................ .......................... .......................... See footnote,3

p.1. 

GC/MS ............. 625,5 1625B ..... 6410 B–00.

HPLC ................ 605.

8. Benzo(a)anthracene .......................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

9. Benzo(a)pyrene ................................................. GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

10. Benzo(b)fluoranthene ...................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

11. Benzo(g,h,i)perylene ........................................ GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

12. Benzo(k)fluoranthene ...................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

13. Benzylchloride ................................................. GC .................... ........................... .......................... .......................... See footnote,3

p. 130. 

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TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued 

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

GC/MS ............. ........................... .......................... .......................... See footnote,6

p. S102. 

14. Butyl benzyl phthalate ..................................... GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

15. Bis(2-chloroethoxy) methane ........................... GC .................... 611.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

16. Bis(2-chloroethyl) ether ................................... GC .................... 611.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

17. Bis(2-ethylhexyl) phthalate .............................. GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

18. Bromodichloromethane .................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

19. Bromoform ....................................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

20. Bromomethane ................................................ GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

21. 4-Bromophenyl phenyl ether ........................... GC .................... 611.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

22. Carbon tetrachloride ........................................ GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

23. 4-Chloro-3-methylphenol ................................. GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

24. Chlorobenzene ................................................ GC .................... 601, 602 ........... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

25. Chloroethane ................................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

26. 2-Chloroethylvinyl ether ................................... GC .................... 601.

GC/MS ............. 624, 1624B.

27. Chloroform ....................................................... GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

28. Chloromethane ................................................ GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

29. 2-Chloronaphthalene ....................................... GC .................... 612 .................... 6410 B–00.

GC/MS ............. 625, 1625B ....... .......................... .......................... See footnote,9

p. 27. 

30. 2-Chlorophenol ................................................ GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

31. 4-Chlorophenyl phenyl ether ........................... GC .................... 611.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

32. Chrysene ......................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

33. Dibenzo(a,h)anthracene .................................. GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

34. Dibromochloromethane ................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

35. 1,2-Dichlorobenzene ........................................ GC .................... 601,602 ............. 6200 C–97.

GC/MS ............. 624, 1625B ....... 6200 B–97 ........ .......................... See footnote,9

p. 27. 

36. 1,3-Dichlorobenzene ........................................ GC .................... 601, 602 ........... 6200 C–97.

GC/MS ............. 624, 1625B ....... 6200 B–97 ........ .......................... See footnote,9

p. 27. 

37. 1,4-Dichlorobenzene ........................................ GC .................... 601, 602 ........... 6200 C–97.

GC/MS ............. 624, 1625B ....... 6200 B–97 ........ .......................... See footnote,9

p. 27. 

38. 3,3-Dichlorobenzidine ...................................... GC/MS ............. 625, 1625B ....... 6410 B–00.

HPLC ................ 605.

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TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued 

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

39. Dichlorodifluoromethane .................................. GC .................... 601.

GC/MS ............. ........................... 6200 C–97.

40. 1,1-Dichloroethane .......................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

41. 1,2-Dichloroethane .......................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

42. 1,1-Dichloroethene .......................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

43. trans-1,2-Dichloroethene ................................. GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

44. 2,4-Dichlorophenol ........................................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

45. 1,2-Dichloropropane ........................................ GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

46. cis-1,3-Dichloropropene ................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

47. trans-1,3-Dichloropropene ............................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

48. Diethyl phthalate .............................................. GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

49. 2,4-Dimethylphenol .......................................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

50. Dimethyl phthalate ........................................... GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

51. Di-n-butyl phthalate ......................................... GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

52. Di-n-octyl phthalate .......................................... GC .................... 606.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

53. 2,3-Dinitrophenol ............................................. GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00.

54. 2,4-Dinitrotoluene ............................................ GC .................... 609.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

55. 2,6-Dinitrotoluene ............................................ GC .................... 609.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... 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–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

58. Fluoranthene .................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

59. Fluorene ........................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

60. 1,2,3,4,6,7,8-Heptachloro-dibenzofuran .......... GC/MS ............. 1613B.

61. 1,2,3,4,7,8,9-Heptachloro-dibenzofuran .......... GC/MS ............. 1613B.

62. 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin ...... GC/MS ............. 1613B.

63. Hexachlorobenzene ......................................... GC .................... 612.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

64. Hexachlorobutadiene ....................................... GC .................... 612.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

65. Hexachlorocyclopentadiene ............................. GC .................... 612.

GC/MS ............. 625,5 1625B ..... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

66. 1,2,3,4,7,8-Hexachlorodibenzofuran ................ GC/MS ............. 1613B.

67. 1,2,3,6,7,8-Hexachlorodibenzofuran ................ GC/MS ............. 1613B.

68. 1,2,3,7,8,9-Hexachlorodibenzofuran ................ GC/MS ............. 1613B.

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58057 

TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued 

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

69. 2,3,4,6,7,8-Hexachlorodibenzofuran ................ GC/MS ............. 1613B.

70. 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin .......... GC/MS ............. 1613B.

71. 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin .......... GC/MS ............. 1613B.

72. 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin .......... GC/MS ............. 1613B.

73. Hexachloroethane ............................................ GC .................... 612.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

74. Ideno(1,2,3-cd) pyrene .................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

75. Isophorone ....................................................... GC .................... 609.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

76. Methylene chloride .......................................... GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

77. 2-Methyl-4,6-dinitrophenol ............................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

78. Naphthalene .................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00.

79. Nitrobenzene ................................................... GC .................... 609.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ ........................... .......................... D4657–92 (99).

80. 2-Nitrophenol ................................................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

81. 4-Nitrophenol ................................................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

82. N-Nitrosodimethylamine .................................. GC .................... 607.

GC/MS ............. 625 5, 1625B ..... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

83. N-Nitrosodi-n-propylamine ............................... GC .................... 607.

GC/MS ............. 6255, 1625B ..... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

84. N-Nitrosodiphenylamine .................................. GC .................... 607.

GC/MS ............. 625 5, 1625B ..... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

85. Octachlorodibenzofuran ................................... GC/MS ............. 1613B10.

86. Octachlorodibenzo-p-dioxin ............................. GC/MS ............. 1613B10.

87. 2,2′-Oxybis(2-chloropropane) [also known as 

bis(2-chloroisopropyl) ether].

GC .................... 611.

GC/MS ............. 625, 1625B ....... 6410 B–00.

88. PCB–1016 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8

GC/MS ............. 625 .................... 6410 B–00.

89. PCB–1221 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8

GC/MS ............. 625 .................... 6410 B–00.

90. PCB–1232 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8

GC/MS ............. 625 .................... 6410 B–00.

91. PCB–1242 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8

GC/MS ............. 625 .................... 6410 B–00.

92. PCB–1248 ....................................................... GC .................... 608.

GC/MS ............. 625 .................... 6410 B–00.

93. PCB–1254 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8

GC/MS ............. 625 .................... 6410 B–00.

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

58058 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued 

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

94. PCB–1260 ....................................................... GC .................... 608 .................... .......................... .......................... See footnote,3

p. 43; See 

footnote.8. 

GC/MS ............. 625 .................... 6410 B–00.

95. 1,2,3,7,8-Pentachloro-dibenzofuran ................ GC/MS ............. 1613B.

96. 2,3,4,7,8-Pentachloro-dibenzofuran ................ GC/MS ............. 1613B.

97. 1,2,3,7,8,-Pentachlorodibenzo-p-dioxin ........... GC/MS ............. 1613B.

98. Pentachlorophenol ........................................... GC .................... 604 .................... 6420 B–00 ........ .......................... See footnote,3

p. 140. 

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

99. Phenanthrene .................................................. GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

100. Phenol ............................................................ GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

101. Pyrene ........................................................... GC .................... 610.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

HPLC ................ 610 .................... 6440 B–00 ........ D4657–92 (99).

102. 2,3,7,8-Tetra-chlorodibenzofuran .................. GC/MS ............. 1613B.

103. 2,3,7,8-Tetra-chlorodibenzo-p-dioxin ............. GC/MS ............. 613, 625,5a

1613B.

104. 1,1,2,2-Tetra-chloro ethane ........................... GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

105. Tetrachloroethene .......................................... GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

106. Toluene .......................................................... GC .................... 602 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

107. 1,2,4-Trichlorobenzene .................................. GC .................... 612 .................... .......................... .......................... See footnote,3

p. 130. 

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

108. 1,1,1-Trichloroethane ..................................... GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

109. 1,1,2-Trichloroethane ..................................... GC .................... 601 .................... 6200 C–97 ....... .......................... See footnote,3

p. 130. 

GC/MS ............. 624, 1624B ....... 6200 B–97.

110. Trichloroethene .............................................. GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

111. Trichlorofluoromethane .................................. GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624 .................... 6200 B–97.

112. 2,4,6-Trichlorophenol ..................................... GC .................... 604 .................... 6420 B–00.

GC/MS ............. 625, 1625B ....... 6410 B–00 ........ .......................... See footnote,9

p. 27. 

113. Vinyl chloride ................................................. GC .................... 601 .................... 6200 C–97.

GC/MS ............. 624, 1624B ....... 6200 B–97.

114. Nonylphenol ................................................... GC/MS ............. ........................... .......................... D7065–06.

LC/MS/MS ........ ........................... .......................... D7485–09.

115. Bisphenol A (BPA) ......................................... GC/MS ............. ........................... .......................... D7065–06.

LC/MS/MS ........ ........................... .......................... D7574–09.

116. p-tert-Octylphenol (OP) ................................. GC/MS ............. ........................... .......................... D7065–06.

LC/MS/MS ........ ........................... .......................... D7485–09.

117. Nonylphenol Monoethoxylate (NP1EO) ........ GC/MS ............. ........................... .......................... D7065–06.

LC/MS/MS ........ ........................... .......................... D7485–09.

118. Nonylphenol Diethoxylate (NP2EO) .............. GC/MS ............. ........................... .......................... D7065–06.

LC/MS/MS ........ ........................... .......................... D7485–09.

119. Polybrominated diphenyl ethers (PBDEs) 49 

congeners.

HRGC/HRMS ... 1614A.

120. Polychlorinated biphenyls (PCBs) 209 

Congeners.

HRGC/HRMS ... 1668C.

121. Adsorbable Organic Halides (AOX) .............. Adsorption and 

Coulometric 

Titration.

1650.

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58059 

TABLE IC—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS—Continued 

Parameter 1 Method EPA2 7 Standard 

methods ASTM Other 

122. Chlorinated Phenolics .................................... In Situ 

Acetylation 

and GC/MS.

1653.

Table IC notes: 

1All parameters are expressed in micrograms per liter (μg/L) except for Method 1613B in which the parameters are expressed in picograms 

per liter (pg/L). 2The full text of Methods 601–613, 624, 625, 1624B, and 1625B, are given at Appendix A, ‘‘Test Procedures for Analysis of Organic Pollutants,’’ of this Part 136. The full text of Method 1613B is incorporated by reference into this Part 136 and is available from the National Technical 

Information Services as stock number PB95–104774. 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. The full text of Methods 1613B, 1614A, 1650, 1653, and 1668C are available from EPA Office of Water (4303T) 1200 Pennsylvannia Ave, 

NW, Washington, DC 20460. 3 ‘‘Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,’’ U.S. Environmental 

Protection Agency, September, 1978. 4 Method 624 may be used for definitive determination of Acrolein and Acrylonitrile. 

5 Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, 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 625, screening only. 6 ‘‘Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,’’ Supplement to the Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater (1981). 7Each 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 (See Appendix A of this Part 136) 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 Empore TM Disk’’ 3M Corporation Revised 10/28/94. 9 USGS Method 0–3116–87 from ‘‘Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments,’’ U.S. Geological Survey, Open File Report 93–125. 10Analysts 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. 

TABLE ID—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1

Parameter Method EPA2 7 10 Standard 

methods ASTM Other 

1. Aldrin ....................... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812–96 

(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

2. Ametryn ................... GC .................... 507, 619 ......................... .......................... .......................... See footnote,3 p. 83; See footnote,9 O–3106–93; See footnote,6 p. S68. 

GC/MS .............. 525.1, 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. a-BHC ...................... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,8

3M0222. 

GC/MS .............. 625 5 ............................... 6410 B–00 ....... .......................... See footnote,11 O–1126–95. 

9. b-BHC ...................... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,8 3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

10. d-BHC .................... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,8 3M0222. 

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

58060 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE ID—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued 

Parameter Method EPA2 7 10 Standard 

methods ASTM Other 

GC/MS .............. 625 .................................. 6410 B–00.

11. g-BHC (Lindane) .... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 5 ............................... 6410 B–00 ....... .......................... See footnote,11 O–1126–95. 

12. Captan ................... GC .................... 617 .................................. 6630 B–00 ....... D3086–90, 

D5812– 

96(02).

See footnote,3 p. 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–00 ....... .......................... See footnote,6 p. S73. 

15. Chlordane .............. GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

16. Chloropropham ...... TLC ................... ......................................... .......................... .......................... See footnote,3 p. 104; See footnote,6 p. S64. 

HPLC ................ 632.

17. 2,4-D ...................... GC .................... 615 .................................. 6640 B–01 ....... .......................... 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–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3105–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

19. 4,4′-DDE ................ GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00. ...... .......................... See footnote,11 O–1126–95. 

20. 4,4′–DDT ............... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

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 .............. 525.1, 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,6 p. S73. 

26. Dichloran ............... GC .................... 608.2, 617 ...................... 6630 B–00 ....... .......................... See footnote,3 p. 7. 

27. Dicofol .................... GC .................... 617 .................................. 6630 B–00 ....... .......................... See footnote,4 O–3104–83. 

28. Dieldrin .................. GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 625 .................................. 6410 B–00 ....... .......................... See footnote,11 O–1126–95. 

29. Dioxathion .............. GC .................... 614.1, 1657 .................... .......................... .......................... See footnote,6 p. S73. 

30. Disulfoton ............... GC .................... 507, 614, 622, 1657 ....... .......................... .......................... See footnote,3 p. 25; See footnote,6 p. S51. 

GC/MS .............. 525.1, 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. 

32. Endosulfan I .......... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M022. 

GC/MS .............. 625 5 ............................... 6410 B–00 ....... .......................... See footnote,13 O–2002–01. 

33. Endosulfan II ......... GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,8

3M0222. 

GC/MS .............. 625 5 ............................... 6410 B–00 ....... .......................... See footnote,13 O–2002–01. 

34. Endosulfan Sulfate GC .................... 608, 617 ......................... 6630 C–00 ....... .......................... See footnote,8 3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

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TABLE ID—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued 

Parameter Method EPA2 7 10 Standard 

methods ASTM Other 

35. Endrin .................... GC .................... 505, 508, 608, 617, 1656 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 525.1, 525.2, 625 5 ......... 6410 B–00.

36. Endrin aldehyde .... GC .................... 608, 617 ......................... 6630 C–00 ....... .......................... See footnote,8 3M0222. 

GC/MS .............. 625.

37. Ethion .................... GC .................... 614, 614.1,1657 ............. .......................... .......................... 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, 1656 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,8

3M0222. 

GC/MS .............. 525.1, 525.2, 625 ........... 6410 B–00.

41. Heptachlor epoxide GC .................... 608, 617 ......................... 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7; See footnote,4

O–3104–83; See footnote,6 p. 

S73; See footnote,8 3M0222. 

GC/MS .............. 625 .................................. 6410 B–00.

42. Isodrin .................... GC .................... 617 .................................. 6630 B–00 & 

C–00.

.......................... 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–00 ....... .......................... 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, 

1656.

6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 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–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 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–00 ....... .......................... See footnote,3 p. 25. 

GC/MS .............. ......................................... .......................... .......................... See footnote,11 O–1126–95. 

53. Parathion ethyl ...... GC .................... 614 .................................. 6630 B–00 ....... .......................... See footnote,3 p. 25. 

GC/MS .............. ......................................... .......................... .......................... See footnote,11 O–1126–95. 

54. PCNB ..................... GC .................... 608.1, 617 ...................... 6630 B–00 ....... D3086–90, 

D5812– 

96(02).

See footnote,3 p. 7. 

55. Perthane ................ GC .................... 617 .................................. 6630 B–00 ....... D3086–90, 

D5812– 

96(02).

See footnote,4 O–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 .............. 525.1, 525.2 ................... .......................... .......................... See footnote,11 O–1126–95. 

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58062 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE ID—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued 

Parameter Method EPA2 7 10 Standard 

methods ASTM Other 

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–00 & 

C–00.

.......................... 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–01 ....... .......................... See footnote,3 p. 115; See footnote,4 O–3105–83. 

67. 2,4,5-TP (Silvex) .... GC .................... 615 .................................. 6640 B–01 ....... .......................... 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, 1656 6630 B–00 & 

C–00.

D3086–90, 

D5812– 

96(02).

See footnote,3 p. 115; See footnote,4 O–3105–83. 

GC/MS .............. 525.1, 525.2, 625 ........... 6410 B–00.

70. Trifluralin ................ GC .................... 508, 617, 627, 1656 ....... 6630 B–00 ....... .......................... See footnote,3 p. 7; See footnote,9

O–3106–93. 

GC/MS .............. 525.1, 525.2 ................... .......................... .......................... See footnote,11 O–1126–95. 

Table ID notes: 

1Pesticides 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. 2The full text of Methods 608 and 625 are given 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,’’ U.S. Environmental 

Protection Agency, September 1978. This EPA publication includes thin-layer chromatography (TLC) methods. 4 ‘‘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 (1987). 5The method may be extended to include a–BHC, g–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 Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater (1981). 7Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 

and 625 (See Appendix A of this Part 136) 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 EmporeTM Disk’’, 3M Corporation, Revised 10/28/94. 9 USGS Method 0–3106–93 from ‘‘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’’ U.S. Geological Survey Open 

File Report 94–37. 10EPA 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. 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58063 

11O–1126–95 GC/MS: Zaugg, S.D., Sandstrom, M.W., Smith, S.G., and Fehlberg, K.M., 1995, 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: U.S. Geological Survey Open-File Report 95–181, Method O–1126–95, 49 p. 12O–2060–01 LC/MS: Furlong, E.T., Anderson, B.D., Werner, S.L., Soliven, P.P., Coffey, L.J., and Burkhardt, M.R., 2001, 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: U.S. Geological Survey Water-Resources Investigations Report 

01–4134 Method O–2060–01, 73 p. 13O–2002–01 Sandstrom, M.W., Stroppel, M.E., Foreman, W.T., and Schroeder, M.P., 2001, 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: U.S. Geological Survey Water-Resources Investigations Report 01–4098, Method O–2002–01, 70 p. 14O–1121–91: Sandstrom, M.W., Wydoski, D.S., Schroeder, M.P., Zamboni, J.L., and Foreman, W.T., 1992, 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,: U.S. Geological Survey Open-File Report 91–519; O–1121– 

91, 34 p. 

* * * * * 

TABLE IG—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS

[40 CFR 455] 

EPA survey 

code Pesticide name CAS No. EPA analytical method No.(s) 

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 [2,4-Dichloro-phenoxyacetic acid].94–75–7 1658/515.1/615/515.2/555 

17 ................... 2,4-DB; 2,4-DB Salts and Esters [2,4- 

Dichlorophenoxybutyric acid].

94–82–6 1658/515.1/615/515.2/555 

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-Methyl-4- 

chlorophenoxyacetic acid].

94–74–6 1658/615/555 

30 ................... Dichlorprop; Dichlorprop Salts and Esters [2-(2,4- 

Dichlorophenoxy) propionic acid].

120–36–5 1658/515.1/615/515.2/555 

31 ................... MCPP; MCPP Salts and Esters [2-(2-Methyl-4- 

chlorophenoxy) propionic acid].

93–65–2 1658/615/555 

35 ................... TCMTB [2-(Thiocyanomethylthio) benzo-thiazole] ....... 21564–17–0 637 

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 ........................................................................ 834–12–8 507/619/525.1/525.2 

60 ................... Atrazine ......................................................................... 1912–24–9 505/507/619/525.1/525.2/1656 

62 ................... Benomyl ........................................................................ 17804–35–2 631 

68 ................... Bromacil; Bromacil Salts and Esters ............................ 314–40–9 507/633/525.1/525.2/1656 

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 1657/507/614/622/525.1/525.2 

107 ................. Parathion methyl ........................................................... 298–00–0 1657/614/622 

110 ................. DCPA [Dimethyl 2,3,5,-tetrachloro-terephthalate] ........ 1861–32–1 508/608.2/525.1/525.2/515.1/515.2/1656 

112 ................. Dinoseb ......................................................................... 88–85–7 1658/515.1/615/515.2/555 

113 ................. Dioxathion ..................................................................... 78–34–2 1657/614.1 

118 ................. Nabonate [Disodium cyanodithio-imidocarbonate] ....... 138–93–2 630.1 

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 Note 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) glycine] ................. 1071–83–6 547 

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58064 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

TABLE IG—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS—Continued 

[40 CFR 455] 

EPA survey 

code Pesticide name CAS No. EPA analytical method No.(s) 

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 11656/1627 

182 ................. Fensulfothion ................................................................ 115–90–2 1657/622 

183 ................. Disulfoton ...................................................................... 298–04–4 1657/507/614/622/525.1/525.2 

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 dimethyldithiocarbamate] .......... 128–03–0 630/630.1 

219 ................. Busan 40 [Potassium N-hydroxymethyl-Nmethyldithiocarbamate].51026–28–9 630/630.1 

220 ................. KN Methyl [Potassium N-methyl-dithiocarbamate] ....... 137–41–7 630/630.1 

223 ................. Prometon ...................................................................... 1610–18–0 507/619/525.1/525.2

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 phosphorotrithioate] ..................... 78–48–8 1657 

239 ................. Simazine ....................................................................... 122–34–9 505/507/619/525.1/525.2/1656 

241 ................. Carbam-S [Sodium dimethyldithiocarbanate] ............... 128–04–1 630/630.1 

243 ................. Vapam [Sodium methyldithiocarbamate] ...................... 137–42–8 630/630.1 

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 phosphorotrithioate] ......................... 150–50–5 1657/507/525.1/525.2/622 

264 ................. Trifluralin ....................................................................... 1582–09–8 1656/508/617/627/525.1/525.2 

268 ................. Ziram [Zinc dimethyldithiocarbamate] .......................... 137–30–4 630/630.1 

1 Monitor and report as total Trifluralin. 

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 per 100 

mL or number per 

gram dry weight.

Most Probable Number 

(MPN), 5 tube, 3 dilution, or.

p. 132 3 ..... 9221 C E–2006.

Membrane filter (MF) 2, 

single step.

p. 124 3 ..... 9222 D–1997 ............... B–0050–85.4

2. Coliform (fecal) in 

presence of chlorine, number per 

100 mL.

MPN, 5 tube, 3 dilution, 

or.

p. 132 3 ..... 9221 C E–2006.

MF 2, single step .......... p. 124 3 ..... 9222 D–1997.

3. Coliform (total), 

number per 100 

mL.

MPN, 5 tube, 3 dilution, 

or.

p. 114 3 ..... 9221 B–2006.

MF 2, single step or two 

step.

p. 108 3 ..... 9222 B–1997 ................ B–0025–85.4

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TABLE IH—LIST OF APPROVED MICROBIOLOGICAL METHODS FOR AMBIENT WATER—Continued 

Parameter and units Method 1 EPA Standard methods AOAC, ASTM, USGS Other 

4. Coliform (total), in 

presence of chlorine, number per 

100 mL.

MPN, 5 tube, 3 dilution, 

or.

p. 114 3 ..... 9221 B–2006.

MF 2 with enrichment ... p. 111 3 ..... 9222 (B+B.5c)–1997.

5. E. coli, number 

per 100 mL.

MPN 6 8 14, multiple tube ................... 9221 B.1–2006/9221 

F–2006.11 13

Multiple tube/multiple 

well.

................... 9223 B–2004 12 ............ 991.15 10 ...................... Colilert®.12 16

Colilert-18®.12 15 16

MF 25678, two step, or 1103.1 19 ... 9222 B–1997/9222 G– 

1997,18 9213 D–1997.

D5392–93.9

Single step ................... 1603 20, 

1604 21.

9213 D–2007 ............... ...................................... mColiBlue-24®.17

6. Fecal 

streptococci, number per 100 mL.

MPN, 5 tube, 3 dilution, p. 139 3 ..... 9230 B–2007.

MF 2, or ........................ p. 136 3 ..... 9230 C–2007 ............... B–0055–85.4

Plate count ................... p. 143.3

7. Enterococci, number per 100 mL.MPN 6 8, multiple tube .. ................... 9230 B–2007.

Multiple tube/multiple 

well.

................... ...................................... D6503–99 9 .................. Enterolert®.12 22

MF 25678 two step ....... 1106.1 23 ... 9230 C–2007 ............... D5259–92.9

Single step, or .............. 1600.24

Plate count ................... p. 143.3

Protozoa: 

8. Cryptosporidium .. Filtration/IMS/FA .......... 1622,25

1623.26

9. Giardia ................ Filtration/IMS/FA .......... 1623.26

1The method must be specified when results are reported. 

2A 0.45 μm 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 USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati, OH. EPA/600/8–78/017. 4 USGS. 1989. 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, U.S. Geological Survey, U.S. Department of the Interior, Reston, VA. 5Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be 

required to resolve any controversies. 6Tests 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. 7When 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. 8To 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. 9ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. ASTM International. 100 

Barr Harbor Drive, West Conshohocken, PA 19428. 10AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical 

Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877–2417. 11The multiple-tube fermentation test is used in 9221B.1. 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. 12These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme b-glucuronidase produced by E. coli. 13After prior enrichment in a presumptive medium for total coliform using 9221B.1, 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. Commercially available EC–MUG media or EC media supplemented in the laboratory with 50 μg/mL of MUG may be used. 14Samples 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® may be enumerated with the multiple-well procedures, Quanti-Tray® or Quanti-Tray®/2000, and the MPN calculated from the table provided by the manufacturer. 15 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of 

incubation at 35 °C rather than the 24 h required for the Colilert® test and is recommended for marine water samples. 16 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories Inc. 1 IDEXX 

Drive, Westbrook, ME 04092. 17A description of the mColiBlue24® test may be obtained from Hach Company, 100 Dayton Ave., Ames, IA 50010. 18Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA–MUG media. 19 USEPA. March 2010. Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–10–002. 20 USEPA. December 2009. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant 

Escherichia coli Agar (Modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–09–007. 21Preparation 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 USEPA. September 

2002.: Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA 821–R–02–024. 

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58066 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

22A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc. 1 IDEXX Drive, Westbrook, ME 04092. 23 USEPA. December 2009. Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar 

(mE–EIA). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–09–015. 24 USEPA. December 2009. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b–D–Glucoside Agar (mEI). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–09–016. 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. USEPA. December 2005. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, 

Office of Water, Washington, DC EPA–821–R–05–001. 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. USEPA. December 2005. Method 1623. Cryptosporidium and Giardia in 

Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–05–002. 

* * * * * 

(b) * * * 

(1) The full texts of the CWA U.S. 

EPA methods are available at http:// 

epa.gov/waterscience/methods/method. 

The full text for determining the method 

detection limit when using the test 

procedures is given in appendix B of 

this part 136. 

* * * * * 

(54) USEPA. March 2010. Method 

1103.1: Escherichia coli (E. coli) in 

Water by Membrane Filtration Using 

membrane-Thermotolerant Escherichia 

coli Agar (mTEC). U.S. Environmental 

Protection Agency, Office of Water, 

Washington, DC EPA–621–R–10–002. 

Available at http://www.epa.gov/

waterscience/methods/method. Table 

IH, Note 19. 

(55) USEPA. December 2009. Method 

1106.1: Enterococci in Water by 

Membrane Filtration Using membraneEnterococcus-Esculin Iron Agar (mE– 

EIA). U.S. Environmental Protection 

Agency, Office of Water, Washington, 

DC EPA–621–R–09–015. Available at 

http://www.epa.gov/waterscience/

methods/method. Table IH, Note 23. 

(56) USEPA. December 2009. Method 

1603: Escherichia coli (E. coli) in Water 

by Membrane Filtration Using Modified 

membrane-Thermotolerant Escherichia 

coli Agar (Modified mTEC). U.S. 

Environmental Protection Agency, 

Office of Water, Washington, DC EPA– 

821–R–09–007. Available at http:// 

www.epa.gov/waterscience/methods/

method. Table IA, Note 20; Table IH, 

Note 20. 

* * * * * 

(59) USEPA. December 2009. Method 

1600: Enterococci in Water by 

Membrane Filtration Using membraneEnterococcus Indoxyl-b-D-Glucoside 

Agar (mEI). U.S. Environmental 

Protection Agency, Office of Water, 

Washington, DC EPA–821–R–09–016. 

Available at http://www.epa.gov/

waterscience/methods/method. Table 

IA, Note 23; Table IH, Note 24. 

(60) USEPA. December 2005. Method 

1622: Cryptosporidium in Water by 

Filtration/IMS/FA. U.S. Environmental 

Protection Agency, Office of Water, 

Washington, DC EPA–821–R–05–001. 

Available at http://www.epa.gov/

waterscience/methods/method. Table 

IA, Note 25. 

(61) USEPA. December 2005. Method 

1623: Cryptosporidium and Giardia in 

Water by Filtration/IMS/FA. U.S. 

Environmental Protection Agency, 

Office of Water, Washington, DC EPA– 

821–R–05–002. Available at http:// 

www.epa.gov/waterscience/methods/ 

method. Table IA, Note 26. 

* * * * * 

(70) USEPA. April 2010. Method 

1680: Fecal Coliforms in Sewage Sludge 

(Biosolids) by Multiple-Tube 

Fermentation using Lauryl Tryptose 

Broth (LTB) and EC Medium. U.S. 

Environmental Protection Agency, 

Office of Water, Washington, DC EPA– 

821–R–10–003. Available at http:// 

www.epa.gov/waterscience/methods/ 

method. Table IA, Note 13. 

* * * * * 

(73) EPA Method 200.5, Revision 4.2. 

‘‘Determination of Trace Elements in 

Drinking Water by Axially Viewed 

Inductively Coupled Plasma-Atomic 

Emission Spectrometry.’’ 2003. EPA/ 

600/R–06/115. (Available at http:// 

www.epa.gov/nerlcwww/ordmeth.htm.) 

* * * * * 

(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 this table takes 

precedence over information provided 

in specific methods or elsewhere unless 

a party documents the acceptability of 

an alternative to the Table II 

instructions. Such alternatives may 

include a change from the prescribed 

preservation techniques, container 

materials, and maximum holding times 

applicable to samples collected from a 

specific discharge. The nature and 

extent of the documentation of such 

changes (how to apply as well as 

supporting data) is left to the discretion 

of the permitting authority (state agency 

or EPA region) or other authority and 

may rely on instructions, such as those 

provided for method modifications at 

§ 136.6. 

TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES

Parameter number/name Container 1 Preservation 2 3

Maximum 

holding time 

(in hours) 4

Table IA—Bacterial Tests: 

1–5. Coliform, total, fecal, and E. coli ................................ PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 23 8 

6. Fecal streptococci .......................................................... PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 8 

7. Enterococci .................................................................... PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 8 

8. Salmonella ..................................................................... PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 8 

Table IA—Aquatic Toxicity Tests: 9–12. Toxicity, acute and 

chronic.

P, FP, G .................................. Cool, 0–6 °C 16 ........................ 36 

*******

Table IH—Bacterial Tests: 

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TABLE II—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued 

Parameter number/name Container 1 Preservation 2 3

Maximum 

holding time 

(in hours) 4

1. E. coli ............................................................................. PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 8 

2. Enterococci .................................................................... PA, G ...................................... Cool, < 10 °C, 0.008% 

Na2S2O3 5.

22 8 

Table IH—Protozoan Tests: 

8. Cryptosporidium ............................................................. LDPE; field filtration ................ 1–10 °C ................................... 21 96 

9. Giardia ............................................................................ LDPE; field filtration ................ 1–10 °C ................................... 21 96 

1 ‘‘P’’ is for polyethylene; ‘‘FP’’ is fluoropolymer (polytetrafluoroethylene (PTFE); Teflon®), 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. 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 °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°, 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 1664A (oil and grease) and the procedures at 40 CFR 

141.34(f)(14)(iv) and (v) (volatile organics). 3When 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). 4Samples 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 (e.g., samples analyzed for fecal coliforms may be held up to 6 hours prior to commencing analysis). 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 °C, with minimum head space. 5ASTM D7365–09a specifies treatment options for samples containing oxidants (e.g. chlorine). 6Sampling, 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. 

* * * * * * * 

16Place 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 °C prior to test initiation. 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. 22Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later than 8 hours from time of collection. 23For 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. 

* * * * * 

4. Section 136.4 is revised to read as 

follows: 

§ 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 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 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 

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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 

(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 Coordinator 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 Coordinators 

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. 

(3) EPA will propose to amend 40 

CFR part 136 to include the alternate 

test procedure in § 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 § 136.5 from the EPA 

Region. 

5. Section 136.5 is revised to read as 

follows: 

§ 136.5 Approval of alternate test 

procedures for limited use. 

(a) Any person may request the 

Regional Alternate Test Procedure 

Coordinator to approved 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. The Director 

will forward the application to the 

Regional Coordinator 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 Table I 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. 

(d) Approval for limited use. (1) After 

a review of the application and in the 

case of a State with an approved NPDES 

permit program, review of the 

recommendation of the Director, the 

Regional Coordinator will notify the 

applicant and the appropriate State 

agency of approval or rejection of the 

use of the alternate procedure. The 

approval may be restricted to use only 

with request to a specific discharge or 

facility (and its laboratory) or, at the 

discretion of the Regional Coordinator, 

to all discharger or facilities (and their 

associated laboratories) specified in the 

approval for the Region. If the 

application for approval is not 

approved, the Regional Coordinator 

shall specify what additional 

information might lead to a 

reconsideration of the application. 

(2) The Regional Coordinator will 

forward a copy of every approval and 

rejection notification to the National 

Alternate Test Procedure Coordinator. 

6. Section 136.6 is revised to read as 

follows: 

§ 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 unmodified 

part 136 method, then the modified 

method is an equivalent and acceptable 

alternative to the approved method. 

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. This documentation should 

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 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58069 

includes analysis of a four replicate 

mid-level standard and a method 

detection limit study. Ongoing quality 

control typically includes method 

blanks, mid-level laboratory control 

samples, and matrix spikes. 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 below. The user 

must notify their permitting authority 

and/or their certification authority/ 

accreditation body of the intent to use 

a modified method when accreditation 

is requested. Such notification should 

be of the form ‘‘Method xxx has been 

modified within the flexibility allowed 

in 40 CFR Part 136.6’’. Specific details 

of the modification need not be 

provided, but must be documented in 

the Standard Operating Procedure 

(SOP). The certification authority/ 

accreditation body may request a copy 

of the SOP. 

(2) Requirements. The modified 

method must have sufficient sensitivity 

to meet the data quality objectives. The 

modified method must also 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’’ or part 

136 method that has such QC, or the 

essential QC requirements specified at 

136.7. If the QC requirements are 

sufficient, but published in other parts 

of an organization’s compendium rather 

than within the part 136 method then 

that part of the organization’s 

compendium must be used. 

(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) Calibration must be performed 

using the modified method. The 

modified method must be tested with 

every wastewater matrix and be applied 

to up to nine distinct matrices in 

addition to any and all reagent water 

tests. If the performance in the 

wastewater matrix or reagent water does 

not meet 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 

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 parameters are not allowed if 

such changes would alter the defined 

methodology (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 preservation 

and/or holding time requirements of an 

approved method. 

(4) Allowable changes. Except as 

noted under Restrictions of this section, 

an analyst may modify an approved test 

procedure (analytical method) provided 

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. These changes refer 

to modifications of the analytical 

procedures used for identification and 

measurement of the analyte and do not 

apply to sample collection and 

preservation procedures. Some 

examples of these types of changes are: 

(A) Use of gas diffusion in place of 

manual or automated distillation. 

(B) 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. 

(C) Interchange of oxidants, such as 

the use of titanium oxide in UV assisted 

automated digestion of TOC and total 

Phosphorus as long as complete 

oxidation can be demonstrated. 

(5) Previously Accepted 

Modifications. The following 

modifications have been used 

successfully in the laboratory 

community for many years. Data have 

demonstrated that these modifications 

provide equivalent performance to the 

methods approved at part 136 across a 

wide variety of matrix types. Therefore, 

these modifications are allowed without 

the need to generate additional 

equivalency data, or the specific 

notification of permitting and/or 

certification authority/accreditation 

bodies required for novel method 

modifications. However, a laboratory 

wishing to use these modifications must 

continue to 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 

§ 136.7. 

(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 

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problems for quantitative determination 

as well as identification based on the 

isotope pattern. Interference reduction 

technologies, such as collision 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. 

(vi) 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 produce 

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 improved. 

(ix) Changes in calibration range 

(provided that the modified range 

covers any relevant regulatory limit.) 

(x) Changes in calibration model. 

Linear calibration models do not 

adequately fit calibration data with one 

or two inflection points. For example, 

vendor-supplied data acquisition and 

processing software provides quadratic 

fitting functions to handle such 

situations. If calibration data for a 

particular analytical method routinely 

display quadratic character, using 

quadratic fitting functions is 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 130.1, cyanide by ASTM D6888 or 

OIA1677, Kjeldahl nitrogen by PAI– 

DK03, and anions by EPA 300.0. When 

a regression curve is calculated 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: 

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. RSE may be used as an alternative 

to correlation coefficients and 

coefficients of determination for 

evaluating calibration curves for any of 

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 RSE is included as an 

alternative to correlation coefficient as a 

measure of the suitability of a 

calibration curve. It is not necessary to 

evaluate both RSE and correlation 

coefficients. 

(xi) Changes in equipment such as 

using similar equipment from a vendor 

different from that mentioned 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 minimum 

detectible concentration. False positives 

are more of a concern when using SIM 

analysis, so at a minimum, one 

quantitation and two qualifying ions 


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must be monitored for each analyte 

(unless less than three ions with 

intensity greater than 15% of the base 

peak are available). The ratio of the two 

qualifying ions to the quantitation ion 

must be evaluated and should agree 

with the ratio of an authentic standard 

within plus/minus 20 percent. Analyst 

judgment must be applied to the 

evaluation of ion ratios since the ratios 

can be affected by co-eluting matrix 

compounds. The signal to noise ratio of 

the least sensitive ion should be at least 

3:1. Retention time should match within 

0.05 minute of an authentic standard 

analyzed under identical conditions. 

Matrix compounds can cause minor 

shifts in retention time and can be 

evaluated by observing any 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 purgeand-trap sample volumes or operating 

conditions. Some examples are: 

(A) Changes in purge time and purgegas flow rate. A change in purge time 

and purge-gas flow rate is allowed 

provided 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 minimum 

detectible concentrations for all 

compounds are met. Using nitrogen as 

a purge gas can provide a significant 

cost saving to the laboratory, compared 

to helium. 

(C) Sample temperature during the 

purge state. Gentle heating of the sample 

during purge (e.g. 40 °C) increases purge 

efficiency of the hydrophilic 

compounds and improves sample-tosample repeatability (%RSD) because all 

samples are purged under precisely the 

same conditions. 

(D) Trap sorbent. Any trap design is 

acceptable provided 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) has no discernable 

effect on compound recoveries, and can 

shorten overall cycle time and 

significantly reduce the amount of water 

introduced to the analytical system 

improving the precision of analysis, 

especially for water soluble analytes. A 

desorb time of four minutes is 

recommended, however a desorb time 

in the range of 0.5–2 minutes 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; an alternate surrogate 

and internal standard concentrations 

other than those specified in the method 

are acceptable provided that method 

performance is not degraded; an 

alternate calibration curve and a 

calibration check other than those 

specified in the method may be used; a 

different solvent for the calibration 

standards may be used to match the 

solvent of the final 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 using salts 

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. Chlorinated samples 

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. Chlorinated samples 

must be dechlorinated prior to the 

addition of such surfactant. 

7. Add new § 136.7 to part 136 to read 

as follows: 

§ 136.7 Quality assurance and quality 

control. 

(a) Twelve essential Quality Control 

checks and acceptable abbreviations are: 

(1) Demonstration of Capability 

(DOC); 

(2) Method Detection Limit (MDL); 

(3) Laboratory reagent blank (LRB), 

also referred to as method blank; 

(4) Laboratory fortified blank (LFB), 

also referred to as a spiked blank, or 

laboratory control sample (LCS); 

(5) Matrix spike, matrix spike 

duplicate, or laboratory fortified blank 

duplicate (LFBD) for suspected difficult 

matrices; 

(6) Internal standards, surrogate 

standards (for organic analysis) or 

tracers (for radiochemistry); 

(7) Calibration (initial and 

continuing), initial and continuing 

performance (ICP) solution also referred 

to as initial calibration verification (ICV) 

and continuing calibration verification 

(CCV); 

(8) Control charts (or other trend 

analyses of quality control results); 

(9) Corrective action (root cause 

analyses); 

(10) QC acceptance criteria; 

(11) Definitions of a batch 

(preparation and analytical); and 

(12) Specify a minimum frequency for 

conducting these QC checks. 

(b) These twelve quality control 

checks must be clearly documented in 

the written method along with a 

performance specification or description 

for each of the twelve quality control 

checks. 

Appendix A [Removed and Reserved] 

8. Remove and reserve Appendix A to 

Part 136. 

Appendix C [Removed and Reserved] 

9. Remove and reserve Appendix C to 

Part 136. 

10. Revise Appendix D to Part 136 to 

read as follows: 

Appendix D to Part 136—Precision and 

Recovery Statement 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 Thallium and 

Zinc. The following precision and 

recovery statements are presented in 

this appendix and incorporated into 

part 136: 

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58072 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

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 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 μg/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, μg/L 

X = Mean Recovery, μg/L 

S = Multi-laboratory Standard Deviation, 

μg/L 

SR = Single-analyst Standard Deviation, 

μg/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 

μg/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, μg/L 

X = Mean Recovery, μg/L 

S = Multi-laboratory Standard Deviation, 

μg/L 

SR = Single-analyst Standard Deviation, 

μg/L 

PART 260—HAZARDOUS WASTE 

MANAGEMENT SYSTEM: GENERAL 

11. 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 

12. Section 260.11 is amended by 

revising paragraph (c)(2) to read as 

follows: 

§ 260.11 References. 

* * * * * 

(c) * * * 

(2) Method 1664, Revision A and 

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, PB99– 

121949 and EPA–821–R–10–001, 

February 2010. IBR approved for part 

261, appendix IX. 

* * * * * 

PART 423—STEAM ELECTRIC POWER 

GENERATING POINT SOURCE 

CATEGORY 

13. 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. 

14. Section 423.11 is amended by 

revising paragraphs (a) and (l) to read as 

follows: 

§ 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 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 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 

15. 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). 

General Provisions 

16. Section 430.01 is amended by 

revising paragraph (a) and by adding 

paragraphs (s) through (v) to read as 

follows: 

§ 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, listed in Table 1C at 40 CFR 136.3. 

* * * * * 

(s) TCDD. 2,3,7,8- 

tetrachlorodibenzop-dioxin. The 

approved method of analysis for TCDD 

is Method 1613B, listed in Table 1C at 

40 CFR 136.3. 

(t) TCDF. 2,3,7,8-tetrachlorodibenzopfuran. The approved method of analysis 

for TCDF is Method 1613B, listed in 

Table 1C at 40 CFR 136.3. 

(u) Chloroform is listed with 

approved methods of analysis in Table 

1C at 40 CFR 136.3. 

(v) The approved method of analysis 

for the following chlorinated phenolic 

compounds is Method 1653, listed in 

Table 1C at 40 CFR 136.3: 

(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. 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58073 

PART 435—OIL AND GAS 

EXTRACTION POINT SOURCE 

CATEGORY 

17. The authority citation for part 435 

continues to read as follows: 

Authority: 33 U.S.C. 1311, 1314, 1316, 

1317, 1318, 1342, and 1361. 

18. Section 435.11 is amended as 

follows: 

a. By revising paragraph (d). 

b. By revising paragraph (e). 

c. By revising paragraph (k)(2). 

d. By revising paragraph (o). 

e. By revising paragraph (t). 

f. By revising paragraph (u). 

g. By revising paragraph (x). 

h. By revising paragraph (ee). 

i. By revising paragraph (gg). 

j. By revising paragraph (hh). 

k. By revising paragraph (ss). 

l. By adding paragraph (uu). 

§ 435.11 Specialized 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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 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 in the ‘‘Analytic Methods for 

the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 in ‘‘Analytic 

Methods for the Oil and Gas Extraction 

Point Source Category,’’ EPA–821–R– 

09–013. 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 in ‘‘Analytic 

Methods for the Oil and Gas Extraction 

Point Source Category,’’ EPA–821–R– 

09–013. See paragraph (uu) of this 

section. 

* * * * * 

(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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 

the ASTM E 1367–92 method: ‘‘Standard 

Guide for Conducting 10-day Static 

Sediment Toxicity Tests with Marine 

and Estuarine Amphipods,’’ 1992, with 

Leptocheirus plumulosus as the test 

organism and sediment preparation 

procedures specified in EPA Method 

1646, which is published in ‘‘Analytic 

Methods for the Oil and Gas Extraction 

Point Source Category,’’ EPA–821–R– 

09–013. See paragraph (uu) of this 

section. 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. 

* * * * * 

(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 in ‘‘Analytic Methods for 

the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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, EPA–821–R–09– 

013, 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 

mstockstill on DSKH9S0YB1PROD with PROPOSALS2

58074 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

Water Docket, 1200 Pennsylvania Ave., 

NW., Washington, DC 20460. 

19. In § 435.12, the first footnote to 

the table is revised to read as follows: 

§ 435.12 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best practicable control technology 

currently available (BPT). 

* * * * * 

BPT EFFLUENT LIMITATIONS—OIL AND

GREASE

*****

*****

1 No discharge of free oil. See § 435.11(x). 

* * * * * 

20. In § 435.13, footnotes 2, 3, and 5 

through 11 to the table are revised to 

read as follows: 

§ 435.13 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best available technology economically 

achievable (BAT). 

* * * * * 

BAT EFFLUENT LIMITATIONS

****

2As determined by the suspended particulate phase (SPP) toxicity test. See 

§ 435.11(gg). 3As determined by the static sheen test. 

See § 435.11(hh). 

* * * * * 

5PAH mass ratio = Mass (g) of PAH (as 

phenanthrene)/Mass (g) of stock base fluid as 

determined by EPA Method 1654, Revision A, 

[specified at § 435.11(u)] entitled ‘‘PAH Content of Oil by HPLC/UV,’’ December 1992, 

which is published in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(uu). 6Base fluid sediment toxicity ratio = 10-day 

LC50 of C16–C18 internal olefin/10-day LC50 of 

stock base fluid as determined by ASTM E 

1367–92 [specified at § 435.11(ee)] method: 

‘‘Standard Guide for Conducting 10-day Static 

Sediment Toxicity Tests with Marine and Estuarine Amphipods,’’ 1992, after preparing the 

sediment according to the procedure specified 

in EPA Method 1646, which is published in 

‘‘Analytic Methods for the Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09– 

013. See § 435.11(uu). 7Biodegradation 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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09–013. See § 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 ASTM E 1367–92 method: 

‘‘Standard Guide for Conducting 10-day Static 

Sediment Toxicity Tests with Marine and Estuarine Amphipods,’’ 1992, with Leptocheirus 

plumulosus as the test organism and sediment 

preparation procedures specified in EPA Method 1646, which is published in ‘‘Analytic Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(ee) and (uu). 9As 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 in ‘‘Analytic 

Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(uu). 10 Maximum permissible retention of nonaqueous drilling fluid (NAF) base fluid on wet 

drill cuttings averaged over drilling intervals 

using NAFs as determined by EPA Method 

1674, which is published in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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 nonaqueous drilling fluid (NAF) base fluid on wet 

drill cuttings averaged over drilling intervals 

using NAFs as determined by EPA Method 

1674, which is published in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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 

ASTM E 1367–92 method: ‘‘Standard Guide 

for Conducting 10-day Static Sediment Toxicity Tests with Marine and Estuarine 

Amphipods,’’ 1992, with Leptocheirus 

plumulosus as the test organism and sediment 

preparation procedures specified in EPA Method 1646, which is published in ‘‘Analytic Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 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 in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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. 

21. In § 435.14, footnote 2 to the table 

is revised to read as follows: 

§ 435.14 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best conventional pollutant control 

technology (BCT). 

* * * * * 

BAT EFFLUENT LIMITATIONS

* * * * 

2 As determined by the static sheen test. 

See § 435.11(hh). 

* * * * * 

22. In § 435.15, footnotes 2, 3, and 5 

through 11 to the table are revised to 

read as follows: 

§ 435.15 Standards of performance for 

new sources (NSPS). 

* * * * * 

NEW SOURCE PERFORMANCE

STANDARDS

* * * * * 

2As determined by the suspended particulate phase (SPP) toxicity test. See 

§ 435.11(gg). 3As determined by the static sheen test. 

See § 435.11(hh). 

* * * * * 

5PAH mass ratio = Mass (g) of PAH (as 

phenanthrene)/Mass (g) of stock base fluid as 

determined by EPA Method 1654, Revision A, 

[specified at § 435.11(u)] entitled ‘‘PAH Content of Oil by HPLC/UV,’’ December 1992, 

which is published in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(uu). 6Base fluid sediment toxicity ratio = 10-day 

LC50 of C16–C18 internal olefin/10-day LC50 of 

stock base fluid as determined by ASTM E 

1367–92 [specified at § 435.11(ee)] method: 

‘‘Standard Guide for Conducting 10-day Static 

Sediment Toxicity Tests with Marine and Estuarine Amphipods,’’ 1992, after preparing the 

sediment according to the procedure specified 

in EPA Method 1646, which is published in 

‘‘Analytic Methods for the Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09– 

013. See § 435.11(uu). 7Biodegradation 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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source Category,’’ EPA–821–R–09–013. See § 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 ASTM E 1367–92 method: 

‘‘Standard Guide for Conducting 10-day Static 

Sediment Toxicity Tests with Marine and Estuarine Amphipods,’’ 1992, with Leptocheirus 

plumulosus as the test organism and sediment 

preparation procedures specified in EPA Method 1646, which is published in ‘‘Analytic Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(ee) and (uu). 

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Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 58075 

9As 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 in ‘‘Analytic 

Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 435.11(uu). 10 Maximum permissible retention of nonaqueous drilling fluid (NAF) base fluid on wet 

drill cuttings averaged over drilling intervals 

using NAFs as determined by EPA Method 

1674, which is published in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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 nonaqueous drilling fluid (NAF) base fluid on wet 

drill cuttings average over drilling intervals 

using NAFs as determined by EPA Method 

1674, which is published in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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 

ASTM E 1367–92 method: ‘‘Standard Guide 

for Conducting 10-day Static Sediment Toxicity Tests with Marine and Estuarine 

Amphipods,’’ 1992, with Leptocheirus 

plumulosus as the test organism and sediment 

preparation procedures specified in EPA Method 1646, which is published in ‘‘Analytic Methods for the Oil and Gas Extraction Point 

Source Category,’’ EPA–821–R–09–013. See 

§ 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 in ‘‘Analytic Methods 

for the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

§ 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. 

23. Subpart A of part 435 is amended 

by removing Appendices 1 through 7. 

24. Subpart A of part 435 is amended 

by redesignating Appendix 8 as 

Appendix 1. 

Subpart D—Coastal Subcategory 

25. Section 435.41 is amended, 

a. By revising paragraph (d). 

b. By revising paragraph (e). 

c. By revising paragraph (k). 

d. By revising paragraph (m)(2). 

e. By revising paragraph (q). 

f. By revising paragraph (r). 

g. By revising paragraph (y). 

h. By revising paragraph (ee). 

i. By revising paragraph (ff). 

j. By adding paragraph (mm). 

§ 435.41 Specialized 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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 in the ‘‘Analytic 

Methods for the Oil and Gas Extraction 

Point Source Category,’’ EPA–821–R– 

09–013. 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 in ‘‘Analytic Methods for the 

Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. 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 in ‘‘Analytic Methods for 

the Oil and Gas Extraction Point Source 

Category,’’ EPA–821–R–09–013. See 

paragraph (mm) of this section. 

(ff) Static sheen test means the 

standard test procedure that has been 

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58076 Federal Register / Vol. 75, No. 184 / Thursday, September 23, 2010 / Proposed Rules 

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 in 

‘‘Analytic Methods for the Oil and Gas 

Extraction Point Source Category,’’ EPA– 

821–R–09–013. 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–09–013, 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. 

26. In § 435.42, footnote 1 to the table 

is revised to read as follows: 

§ 435.42 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best practicable control technology 

currently available (BPT). 

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

* * * * * 

27. In § 435.43, footnotes 2 and 4 are 

revised to read as follows: 

§ 435.43 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best available technology economically 

achievable (BAT). 

* * * * * 

BAT EFFLUENT LIMITATIONS

* * * * * 

2As determined by the static sheen test. 

See § 435.41(ff). 

* * * * * 

4As determined by the suspended particulate phase (SPP) toxicity test. See 

§ 435.41(ee). 

* * * * * 

28. In § 435.44 footnote 2 to the table 

is revised to read as follows: 

§ 435.44 Effluent limitations guidelines 

representing the degree of effluent 

reduction attainable by the application of 

the best conventional pollutant control 

technology (BCT). 

* * * * * 

BAT EFFLUENT LIMITATIONS

* * * * * 

2As determined by the static sheen test. 

See § 435.41(ff). 

* * * * * 

29. In § 435.45, footnotes 2 and 4 to 

the table are revised to read as follows: 

§ 435.45 Standards of performance for 

new sources (NSPS). 

* * * * * 

NSPS EFFLUENT LIMITATIONS

* * * * * 

2As determined by the static sheen test. 

See § 435.41(ff). 

* * * * * 

4As determined by the suspended particulate phase (SPP) toxicity test. See 

§ 435.41(ee). 

* * * * * 

[FR Doc. 2010–20018 Filed 9–22–10; 8:45 am] 

BILLING CODE 6560–50–P 

mstockstill on DSKH9S0YB1PROD with PROPOSALS2