Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6967 

practicable and permitted by law. 

Executive Order 14096 (Revitalizing Our 

Nation’s Commitment to Environmental 

Justice for All, 88 FR 25251, April 26, 

2023) builds on and supplements E.O. 

12898 and defines EJ as among other 

things, the just treatment and 

meaningful involvement of all people 

regardless of income, race, color, 

national origin, or Tribal affiliation, or 

disability in agency decision-making 

and other Federal activities that affect 

human health and the environment. 

South Carolina did not evaluate EJ 

considerations as part of its SIP 

submittal; the CAA and applicable 

implementing regulations neither 

prohibit nor require such an evaluation. 

EPA did not perform an EJ analysis and 

did not consider EJ in this proposed 

action. Due to the nature of the 

proposed action being taken here, this 

proposed action is expected to have a 

neutral to positive impact on the air 

quality of the affected area. 

Consideration of EJ is not required as 

part of this action, and there is no 

information in the record inconsistent 

with the stated goal of E.O. 12898/14096 

of achieving EJ for communities with EJ 

concerns. 

List of Subjects in 40 CFR Part 52 

Environmental protection, Air 

pollution control, Carbon monoxide, 

Incorporation byreference, 

Intergovernmental relations, Lead, 

Nitrogen dioxide, Ozone, Particulate 

matter, Reporting and recordkeeping 

requirements, Sulfur oxides, Volatile 

organic compounds. 

Authority: 42 U.S.C. 7401 et seq. 

Dated: January 6, 2025. 

Jeaneanne Gettle, 

Acting Regional Administrator, Region 4. 

[FR Doc. 2025–00438 Filed 1–17–25; 8:45 am] 

BILLING CODE 6560–50–P 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Part 136 

[EPA–HQ–OW–2024–0328; FRL 11799–01– 

OW] 

RIN 2040–AG37 

Clean Water Act Methods Update Rule 

22 for the Analysis of Contaminants in 

Effluent 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Proposed rule. 

SUMMARY: The U.S. Environmental 

Protection Agency (EPA) is proposing to 

promulgate new methods and update 

the tables of approved methods for the 

Clean Water Act. The Clean Water Act 

requires the EPA to promulgate test 

procedures for the analysis of 

pollutants. Promulgating new methods 

and updating the tables of approved 

methods increases the quality and 

consistency of data collected for the 

purposes of the Clean Water Act. In this 

rule, the EPA proposes to add new EPA 

methods for per- and polyfluoroalkyl 

substances (PFAS) and polychlorinated 

biphenyl (PCB) congeners, and add 

methods previously published by 

voluntary consensus bodies that 

industries and municipalities would use 

for reporting under the EPA’s National 

Pollutant Discharge Elimination System 

permit program. The EPA also proposes 

to withdraw the seven Aroclor (PCB 

mixtures) parameters. In addition, the 

EPA is proposing to simplify the 

sampling requirements for two volatile 

organic compounds, and make a series 

of minor corrections to existing tables of 

approved methods. This proposed rule 

does not mandate when a parameter 

must be monitored or establish a 

discharge limit. 

DATES: Comments must be received on 

or before February 20, 2025. 

ADDRESSES: You may send comments, 

identified by Docket ID No. EPA–HQ– 

OW–2024–0328, by any of the following 

methods: 

• Federal eRulemaking Portal: 

https://www.regulations.gov/ (our 

preferred method). Follow the online 

instructions for submitting comments. 

• Mail: U.S. Environmental 

Protection Agency, EPA Docket Center, 

Office of Water Docket, Mail Code 

28221T, 1200 Pennsylvania Avenue 

NW, Washington, DC 20460. 

• Hand Delivery or Courier: EPA 

Docket Center, WJC West Building, 

Room 3334, 1301 Constitution Avenue 

NW, Washington, DC 20004. The Docket 

Center’s hours of operations are 8:30 

a.m.–4:30 p.m., Monday–Friday (except 

Federal Holidays). 

Instructions: All submissions received 

must include the Docket ID No. for this 

rulemaking. Comments received may be 

posted without change to https://

www.regulations.gov/, including any 

personal information provided. For 

detailed instructions on sending 

comments and additional information 

on the rulemaking process, see the 

‘‘Public Participation’’ heading of the 

SUPPLEMENTARY INFORMATION section of 

this document. 

FOR FURTHER INFORMATION CONTACT: 

Adrian Hanley, Engineering and 

Analysis Division, Office of Water 

(4303T), Environmental Protection 

Agency, 1200 Pennsylvania Avenue 

NW, Washington, DC 20460–0001; 

telephone number: 202–564–1564; 

email address: hanley.adrian@epa.gov. 

SUPPLEMENTARY INFORMATION: Table of 

Contents 

I. Public Participation 

II. General Information 

III. Background 

IV. Corrections or Amendments to the Text 

and Tables of 40 CFR part 136 

V. Incorporation by Reference 

VI. Statutory and Executive Order Reviews 

I. Public Participation 

A. Written Comments 

Submit your comments, identified by 

Docket ID No. EPA–HQ–OW–2024– 

0328, at https://www.regulations.gov 

(our preferred method), or the other 

methods identified in the ADDRESSES

section. Once submitted, comments 

cannot be edited or removed from the 

docket. The EPA may publish any 

comment received to its public docket. 

Do not submit to the EPA’s docket at 

https://www.regulations.gov any 

information you consider to be 

Confidential Business Information (CBI), 

Proprietary Business Information (PBI), 

or other information whose disclosure is 

restricted by statute. Multimedia 

submissions (audio, video, etc.) must be 

accompanied by a written comment. 

The written comment is considered the 

official comment and should include 

discussion of all points you wish to 

make. The EPA will generally not 

consider comments or comment 

contents located outside of the primary 

submission (i.e., on the web, cloud, or 

other file sharing system). Please visit 

https://www.epa.gov/dockets for 

additional submission information; the 

full EPA public comment policy; 

information about CBI, PBI, or 

multimedia submissions; and general 

guidance on making effective 

comments. Publicly available docket 

materials are available electronically in 

https://www.regulations.gov at the 

Water Docket in EPA Docket Center, 

EPA/DC, EPA West William J. Clinton 

Building, Room 3334, 1301 Constitution 

Avenue 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. Any 

copyright material can be viewed at the 

Reading Room, please contact the EPA 

Docket Center, Public Reading Room. 

The telephone number for the Public 

Reading Room is 202–566–1744, and the 

telephone number for the Water Docket 

is 202–566–2426. Fax: 202–566–9744. 

Email: docket-customerservice@epa.gov. 


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6968 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 

1Formerly known as the American Society for 

Testing and Materials (ASTM). 

II. General Information 

A. Does this action apply to me? 

Entities potentially affected by the 

requirements of this action include: 

Category Examples of potentially affected entities 

State, Territorial, and Indian Tribal 

Governments.

States authorized to administer the National Pollutant Discharge Elimination System permitting program; 

states, territories, and Tribes providing certification under CWA section 401; state, territorial, and Tribalowned facilities that must conduct monitoring to comply with NPDES permits. 

Industry ........................................... Facilities that must conduct monitoring to comply with NPDES permits; the environmental monitoring industry. 

Municipalities ................................... Publicly Owned Treatment Works or other municipality-owned facilities that must conduct monitoring to 

comply with NPDES permits. 

This table is not intended to be 

exhaustive, but rather provides a guide 

for readers regarding entities likely to be 

affected by this action. This table lists 

types of entities that the EPA is now 

aware of that could potentially be 

affected by this action. Other types of 

entities not listed in the table could also 

be affected. To determine whether your 

facility is affected by this action, you 

should carefully examine the 

applicability language at 40 CFR 122.1 

(NPDES purpose and scope), 40 CFR 

136.1 (NPDES permits and CWA) and 40 

CFR 403.1 (pretreatment standards 

purpose and applicability). If you have 

questions regarding the applicability of 

this action to a particular entity, consult 

the appropriate person listed in the 

preceding FOR FURTHER INFORMATION

CONTACT section. 

B. What action is the Agency taking? 

Periodically, the EPA updates the 

approved methods in 40 CFR part 136. 

This proposed rulemaking is the 24th 

update to 40 CFR part 136 since its 

inception in 1973, 22 Method Update 

Rules and two Routine Method Update 

Rules. In general, the changes in this 

action fall into six categories. The first 

category is withdrawal of the seven 

Aroclor parameters and associated 

methods. The second category is 

withdrawal of outdated methods that 

have been supplanted by already 

approved methods at 40 CFR part 136. 

The third category is a simplification of 

the sampling and preservation 

requirements for two volatile organic 

compound methods. The fourth 

category includes minor corrections in 

the text and tables in 40 CFR part 136. 

The EPA is proposing these revisions to 

keep current with technology advances, 

and to improve data quality and 

consistency for the regulated 

community. The fifth category is new 

EPA methods for new parameters that 

are being added to 40 CFR part 136. The 

sixth category is new methods 

published by a voluntary consensus 

standard body or vendor for new 

parameters. The following paragraphs 

provide details on the revisions. The 

first four categories are discussed in 

section IV Corrections or Amendments 

to the Text and Tables of 40 CFR part 

136 of this preamble, the fifth and sixth 

categories are discussed in section V 

Incorporation by Reference of this 

preamble. 

C. What is the Agency’s authority for 

taking this action? 

The EPA is proposing this regulation 

under the authorities of sections 301(a), 

304(h), and 501(a) of the CWA; 33 

U.S.C. 1251, 1311(a), 1314(h) and 

1361(a). Section 301(a) of the CWA 

prohibits the discharge of any pollutant 

into navigable waters unless the 

discharge complies with, among other 

provisions, a NPDES permit issued 

under section 402 of the CWA. Section 

304(h) of the CWA requires the EPA 

Administrator 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 the CWA] or permit 

application pursuant to [section 402 of 

the CWA].’’ Section 501(a) of the CWA 

authorizes the EPA Administrator to 

‘‘. . . prescribe such regulations as are 

necessary to carry out this function 

under [the CWA].’’ The EPA generally 

has codified its test procedure 

regulations (including analysis and 

sampling requirements) for CWA 

programs at 40 CFR part 136, though 

some requirements are codified in other 

parts (e.g., 40 CFR Chapter I, 

Subchapters N and O). 

III. Background 

This preamble describes the 

abbreviations and acronyms used, the 

legal authority and reasons for the 

proposed rule, and a summary of the 

proposed changes and clarifications, 

and solicits comment from the public. 

Abbreviations and Acronyms Used in 

the Preamble 

AOF: Adsorbable Organic Fluorine 

ASTM: ASTM International 1

CFR: Code of Federal Regulations 

CWA: Clean Water Act 

EPA: The U.S. Environmental Protection 

Agency 

GC/MS: Gas Chromatography/Mass 

Spectrometry 

H2O2: Hydrogen Peroxide 

ICP/AES: Inductively Coupled PlasmaAtomic Emission Spectroscopy 

LC–MS/MS: Liquid Chromatography-Tandem 

Mass Spectrometry (also used as LC/MS/ 

MS in some methods) 

NPDES: National Pollutant Discharge 

Elimination System 

NTTAA: National Technology Transfer and 

Advancement Act 

PAA: Peracetic Acid 

PCB: Polychlorinated Biphenyl 

PFAS: Per- and Polyfluoroalkyl Substances 

POTW: Publicly Owned Treatment Works 

QC: Quality Control 

TNI: The NELAC Institute 

USGS: United States Geological Survey 

VCSB: Voluntary Consensus Standards Body 

NPDES permits must include 

conditions to ensure compliance with 

the technology-based and water qualitybased requirements of the CWA, 

including in many cases, restrictions on 

the quantity of specific pollutants that 

can be discharged. Permittees must use 

EPA-approved analytical methods that 

are sensitive enough to detect and 

measure pollutants at or below permit 

limits or water quality criteria (CWA 

section 402(b)(2)(A)). Permits include 

measurement and reporting 

requirements for these specific 

pollutants; however, permittees often 

have a choice of which approved test 

procedure they will use when the EPA 

has approved more than one method for 

a specific pollutant. 

The procedures for the analysis of 

pollutants required by CWA section 

304(h) are a central element of the 

NPDES permit program. Examples of 


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2EPA document EPA–600/4–84–061, ‘‘EPA 

Method Study 18 Method 608—Organochlorine 

Pesticides and PCBs.’’ June 1984. 

3EPA document EPA 820–R–21–003, ‘‘Report on 

the Multi-laboratory Validation of Clean Water Act 

Method 1628 for PCB Congeners.’’ April 2021. 

where these EPA-approved analytical 

methods must be used include the 

following: (1) applications for NPDES 

permits, (2) sampling or other reports 

required under NPDES permits, (3) 

other requests for quantitative or 

qualitative effluent data under the 

NPDES regulations, (4) State CWA 401 

certifications, and (5) sampling and 

analysis required under EPA’s General 

Pretreatment Regulations for Existing 

and New Sources of Pollution, 40 CFR 

136.1, 40 CFR 403.12(b)(5)(v), and 40 

CFR 403.12(g)(3). 

Periodically, the EPA promulgates 

updates to the approved methods in 40 

CFR part 136 to improve data quality 

and consistency. The changes proposed 

in this action fall into the following 

categories. The first category is 

withdrawal of seven Aroclor mixtures 

and the associated approved methods 

for Aroclors from the list of parameters 

at Table Ic that have been replaced with 

a method for the PCB congeners and 

total PCBs at Table Ii that provides a 

more accurate and complete 

characterization of the PCB content of 

samples than Aroclor analyses (see 

section V.A of this preamble). The 

second category is withdrawal of 

outdated methods that includes singleanalyte total metal colorimetric methods 

for twelve metal parameters, a WatersTM

anion method, and EPA Method 1664A 

for the parameter ‘‘oil and grease’’ (see 

section IV.B of this preamble). The third 

category is simplifying sampling 

requirements for purgeable compounds 

by making the preservation requirement 

for acrolein and acrylonitrile consistent 

with the other pollutants analyzed by 

volatile organic compound methods (see 

section IV.C of this preamble). The 

fourth category is minor corrections to 

the text and tables at 40 CFR part 136 

(see section IV.D of this preamble). The 

fifth category is new EPA methods for 

new parameters not previously listed at 

40 CFR part 136 that will be added by 

incorporation by reference: per- and 

polyfluoroalkyl substances (PFAS) by 

EPA Method 1633A to a new Table Ij, 

adsorbable organic fluorine (AOF) by 

EPA Method 1621 to Table Ic, and 

polychlorinated biphenyl (PCB) 

congeners by EPA Method 1628 to a 

new Table Ii (see section V.A of this 

preamble). The EPA has finalized these 

three EPA methods and has posted these 

methods, along with their validation 

study reports, on EPA’s CWA Methods 

website (https://www.epa.gov/cwamethods). The sixth category is new 

methods published by the voluntary 

consensus standard bodies (VCSBs) or 

vendors for new parameters not 

previously listed at 40 CFR part 136 that 

will be added by incorporation by 

reference: PFAS analytes by ASTM 

D8421–24 to Table Ij; peracetic acid 

(PAA) by Standard Method ‘‘4500–PAA 

Peracetic Acid (Residual),’’ and 

hydrogen peroxide (H2O2) by Standard 

Method ‘‘4500–H2O2 Hydrogen Peroxide 

(Residual)’’ to Table Ib (see section V.B 

of this preamble). Finally, as a 

consequence of adding the two new 

tables for the PCB congeners and PFAS, 

the format of the numbers for the 

existing Tables IA through IH are being 

revised to be called out as Tables Ia 

through Ih. The use of a lowercase letter 

in the table identifier is necessary to 

avoid confusion between the new Table 

Ii of PCB congeners and the existing 

Table II with the required containers, 

preservation techniques, and holding 

times (see section V.A of this preamble). 

IV. Corrections or Amendments to the 

Text and Tables of 40 CFR Part 136 

A. Withdrawal of the Aroclor 

Parameters and the Associated Methods 

The EPA proposes to withdraw the 

seven Aroclor parameters listed as PCB– 

1016, PCB–1221, PCB–1232, PCB–1242, 

PCB–1248, PCB–1254, and PCB–1260 

and their associated methods from Table 

Ic, Parameters 88–94. Removing these 

parameters will result in the 

renumbering of all of the subsequent 

parameters in that table. This will also 

result in deletion of footnote 8, and the 

renumbering of footnotes 9 through 16. 

All of the methods listed for these 

parameters are listed elsewhere for other 

parameters, so none of them will be 

completely removed from 40 CFR part 

136.3. The ‘‘PCBs’’ class of compounds 

is made up of 209 structurally related 

but distinct chemicals often called 

‘‘congeners.’’ The seven Aroclor 

parameters are commercial PCB 

mixtures and were first included in the 

EPA’s 1976 Priority Pollutant List 

(Appendix A to Part 423, Title 40). 

These seven PCB mixtures were the 

only ones for which the EPA had valid 

methods at that time. However, none of 

these Aroclor mixtures include all the 

PCB congeners that may be present in 

an environmental sample. The EPA 

developed the original Aroclor methods 

in the 1970s, when analysis of 

individual PCB congeners was 

impractical with the existing affordable 

analytical technology and in the absence 

of automated laboratory information 

management systems. During the multilaboratory study of Method 608 in the 

late 1970s, roughly 20% of the Aroclor 

data were rejected due to poor accuracy, 

and false negatives (non-detects) were 

an issue even with samples that were 

spiked with fresh standards.2

When used as a surrogate for PCBs, 

the results from the approved Aroclor 

methods can create false confidence that 

PCBs are not present. Given that the 

manufacturing and use of PCBs have 

been banned in the U.S. since 1979, 

most PCBs in the environment have 

been subjected to extensive changes in 

composition and concentration through 

processes that are collectively referred 

to as ‘‘weathering.’’ Moreover, there are 

other relevant sources of PCBs to the 

environment beyond the seven Aroclor 

parameters that are not accounted for 

through Aroclor analyses. Aroclor 

methods were the best available 

technology when they were validated in 

1978, but now there are much more 

accurate methods. Thus, the EPA is 

proposing to replace the Aroclor 

analysis with EPA Method 1628, which 

detects the 209 PCB congeners directly, 

either as individual congeners or groups 

of co-eluting congeners. As 

demonstrated by the EPA’s multilaboratory study,3 EPA Method 1628 

can be widely implemented because it 

uses laboratory equipment that is 

readily available and is already 

employed by many full-service 

laboratories. 

Withdrawal of the Aroclor parameters 

and associated methods will not have 

any immediate impact on current 

NPDES permits because permits that 

have been issued by the permitting 

authority can continue until they expire. 

40 CFR 122.21(e)(3)(ii) states: ‘‘(ii) When 

there is no analytical method that has 

been approved under 40 CFR part 136, 

required under 40 CFR chapter I, 

subchapter N or O, and is not otherwise 

required by the Director, the applicant 

may use any suitable method but shall 

provide a description of the method. 

When selecting a suitable method, other 

factors such as a method’s precision, 

accuracy, or resolution, may be 

considered when assessing the 

performance of the method.’’ EPA 

anticipates renewed permits will switch 

to the approved PCB congener method. 

Given that most permits are renewed 

every 5 years or less, promulgation of 

this part of this proposed rule would 

result in a multi-year phase out of 

Aroclor analysis. 

B. Withdrawal of Outdated Methods 

The EPA proposes to withdraw 

approval of outdated colorimetric 


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methods for 12 individual metals and 

one inorganic anions alternate test 

procedure that the sponsoring 

organization no longer supports or 

makes available to the public. The 

removal of these methods and their 

associated footnotes will result in 

renumbering of the following footnotes 

at the end of Table Ib. 

1. The EPA proposes to withdraw 12 

single-metal colorimetric methodology 

types that measure a total metal 

concentration (e.g., ‘‘Aluminum— 

Total’’) from 40 CFR 136.3, Table Ib. 

There are multiple inductively coupled 

plasma (ICP) and graphite furnace 

methods that are more sensitive and 

provide more accurate results in 

challenging matrices that are already 

listed in Table Ib. These ICP and 

graphite furnace methods are also 

relatively inexpensive and easily 

automated, particularly when analyzing 

for one parameter (as is done for the 

colorimetric methods that the EPA is 

proposing to withdraw). The suggestion 

to withdraw these methods initially 

came from The NELAC Institute (TNI), 

which accredits a large portion of the 

environmental laboratories in the U.S. 

TNI is unaware of any laboratory that is 

currently accredited for these outdated 

colorimetric methods. If the EPA 

receives compelling reason to not 

withdraw any of these methods, the 

EPA will consider keeping some or all 

of these methods in 40 CFR part 136. 

Otherwise, the EPA proposes to 

withdraw the methods in the rows 

where ‘‘Colorimetric’’ is the listed 

methodology for the following total 

metals, listed in order of the parameter 

number in Table Ib: 3. Aluminum— 

Total, 6. Arsenic—Total, 8. Beryllium— 

Total, 10. Boron—Total, 12. Cadmium— 

Total, 19. Chromium—Total, 22. 

Copper—Total, 30. Iron—Total, 32. 

Lead—Total, 34. Manganese—Total, 74. 

Vanadium—Total, and 75. Zinc—Total. 

In addition, footnotes pertaining to only 

these withdrawals will be removed and 

the remaining footnotes renumbered 

sequentially. The relevant methods that 

will be withdrawn are listed here by 

organization. Standard Methods: 3500- 

Al B–2020, 3500-As B–2020, 4500–B B– 

2011, 3500-Cd D–1990, 3500-Cr B–2020, 

3500-Cu B and C–2020, 3500 Fe B–2011, 

3500-Pb B–2020, 3500-Mn B–2020, 

3500–V B–2011, 3500-Zn B–2020, and 

Footnote 61 that references an aluminon 

colorimetric method in Standard 

Methods 19th Edition. ASTM: D2972– 

15 (A), D1068–15 (C). USGS: Methods I– 

3060–85 and I–3112–85. Hach: Footnote 

19 that references Method 8506, 

Bicinchoninate Method for Copper, 

Hach Handbook of Water Analysis, 

1979; Footnote 22 that references 

Method 8008, 1,10-Phenanthroline 

Method using FerroVer Iron Reagent for 

Water, 1980; Footnote 23 that references 

Method 8034, Periodate Oxidation 

Method for Manganese, Hach Handbook 

of Wastewater Analysis, 1979; and 

Footnote 33 that references Method 

8009, Zincon Method for Zinc, Hach 

Handbook of Water Analysis, 1979. 

AOAC International: Footnote 3 that 

references Method 920.203, the 

persulfate oxidation procedure from the 

Official Methods of Analysis of the 

Association of Official Analytical 

Chemists, Methods Manual, Sixteenth 

Edition, 4th Revision, 1998. 

2. The EPA also proposes to withdraw 

from Table Ib the WatersTM Corporation 

alternate test procedure: ‘‘Method 

D6508 Rev.2, Test Method for 

Determination of Dissolved Inorganic 

Anions in Aqueous Matrices Using 

Capillary Ion Electrophoresis and 

Chromate Electrolyte.’’ The WatersTM

Corporation no longer supports this 

method and no longer provides copies 

of this method to the public. WatersTM

developed their alternative test 

procedure to incorporate additional 

analysis techniques into an older ASTM 

standard. The method modifications 

developed by WatersTM were 

incorporated into later versions of the 

ASTM standard, including D6508–15, 

which is the currently approved method 

for the same anions: bromide, chloride, 

fluoride, nitrate, nitrate-nitrite, nitrite, 

orthophosphate, and sulfate (86 FR 

27226, May 19, 2021). Both the 

WatersTM and ASTM methods are 

capillary ion electrophoresis methods 

that provide a simultaneous separation 

and determination of several inorganic 

anions and identifies all anions present 

in the sample by indirect UV detection. 

The EPA proposes to remove the eight 

occurrences of Method D6508 Rev. 2 

from Table Ib. They are found in 

parameters: 11. Bromide, 16. Chloride, 

25. Fluoride-Total, 38 Nitrate (as N), 39. 

Nitrate-nitrite (as N), 40. Nitrite (as N), 

44. Ortho-phosphate (as P), and 65. 

Sulfate (as SO4). 

3. The EPA proposes to withdraw 

EPA Method 1664, Revision A: NHexane Extractable Material (HEM; Oil 

and Grease) and Silica Gel Treated NHexane Extractable Material (SGTHEM; 

Non-polar Material) by Extraction and 

Gravimetry, approved at 64 FR 26315, 

May 14, 1999, from Table Ib, parameter 

41. A later revision of Method 1664, 

(1664 Rev. B), was approved by the EPA 

in a 2012 rulemaking, 77 FR 29758, May 

18, 2012. That 2012 rule strongly 

recommended laboratories and 

permitting authorities replace Method 

1664, Rev. A with Method 1664, Rev. B. 

The 2012 rule also said that the EPA 

would revisit withdrawing Method 

1664, Rev. A in a future rulemaking (77 

FR 29758, May 18, 2012). Laboratories 

and regulatory entities have had more 

than 12 years to make this adjustment, 

so the EPA is proposing to withdraw 

Method, 1664, Rev. A from Table Ib, for 

parameter 41. Oil and Grease—Total 

recoverable. 

C. Simplify the Sampling and 

Preservation Requirements for Two 

Purgeable Organic Compounds (Often 

Referred to as Volatile Organic 

Compounds) 

The EPA proposes to change the 

sampling and preservation requirements 

for acrolein and acrylonitrile to match 

those of the other purgeable halocarbons 

and purgeable aromatic hydrocarbons in 

Table II under the section for parameters 

in Table Ic. The EPA proposes to change 

the preservation pH requirement from 

pH 4–5 to a pH of 2, and to use 

hydrochloric acid to adjust the sample 

pH, to align with the approved practice 

for other purgeable organic compounds. 

The Environmental Monitoring 

Coalition provided the EPA with the 

results from a study using multiple 

wastewater types that demonstrated that 

the analysis of acrolein and acrylonitrile 

is not adversely affected by the lower 

pH preservation. That Environmental 

Monitoring Coalition study report: 

‘‘Evaluating Preservation Requirements 

for Acrolein and Acrylonitrile in 

Aqueous Matrices,’’ is provided in the 

docket. Thus, the EPA is proposing 

these changes to make the sampling, 

analysis, and data reporting more 

efficient for purgeable organic 

compound methods. 

D. Minor Corrections and Amendments 

to the Texts and Tables of 40 CFR Part 

136 

Stakeholders have identified several 

minor errors in Tables Ib, Id, and II. The 

EPA proposes to correct the following 

entries in those tables. 

1. The EPA proposes to remove the 

row for the methodology 

‘‘Amperometric direct (low level)’’ in 

Table Ib, parameter 17A, Chlorine-Free 

Available, because the only method 

listed in that row, Standard Method 

4500 Cl E, measures Total Residual 

Chlorine (e.g., parameter 17), not free 

chlorine. The method will remain in the 

corresponding row for Residual 

Chlorine parameter 17, where the 

parameter matches the method. 

2. The EPA proposes to amend Table 

Ib parameter 24 by adding 4500–CN P– 

2021 and D7511(17) to allow use of any 

method approved for measurement of 

Total Cyanide in both the untreated and 


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treated fractions of a sample for 

determination of available cyanide by 

cyanide amenable to chlorination 

(CATC), provided the treatment steps in 

the two currently approved amenable 

cyanide methods, 4500–CN G–2016 and 

ASTM D2036–09(15)(B), are followed. 

3. The EPA proposes to add EPA 

Method 625.1 as an approved method 

for the parameter Parathion ethyl, 

parameter 53 in Table Id. The use of 

EPA Method 625.1 was incorrectly 

omitted from Table Id for this parameter 

the last time that Table Id was updated 

(82 FR 40836, August 28, 2017) because 

the method lists this analyte as 

‘‘Parathion,’’ rather than Parathion 

ethyl. EPA Method 625.1 measures 

aqueous samples by extracting them 

with methylene chloride at pH 11—13 

and again at a pH less than 2 using a 

separatory funnel or continuous liquid/ 

liquid extractor. Then the extract is 

concentrated and analyzed by GC/MS. 

4. The EPA proposes to apply footnote 

9 to the entry for EPA Method 1613B in 

Table Ic for parameter 96, 2,3,7,8- 

Tetrachloro-dibenzo-p-dioxin (formerly 

listed a parameter 103). This footnote 

(formerly listed as footnote 10) was to be 

added to all 17 dioxin and furan 

congeners in a previous rule (88 FR 

10739, February 21, 2023) but was 

inadvertently missed for this parameter. 

5. The EPA proposes to add sodium 

thiosulfate, Na2S2O3, to the preservation 

column for parameter 4, Ammonia, 

under Table Ib in Table II, and apply 

Footnote 5 to that entry to address the 

fact that residual chlorine in samples 

will react with ammonia to form 

chloramines, which are an interference 

with ammonia analyses. The EPA also is 

adding the following text to the end of 

Footnote 5, ‘‘Section A.2 of Standard 

Method 4500–NH3 discusses the need 

for dechlorination of samples for 

ammonia analysis.’’ 

6. The EPA proposes to edit Footnote 

17 to Table II under the section for 

parameters in Table Ib, as applied to 

parameter 35 for ‘‘Mercury (CVAFS)’’ to 

include mention of EPA Method 245.7 

along with EPA Method 1631 in the 

footnote. Both methods employ the 

same cold vapor atomic fluorescence 

spectroscopy (CVAFS) determinative 

technique and including EPA Method 

245.7 in the footnote will help clarify 

that the 90-day holding time applies to 

EPA Method 245.7 as well as EPA 

Method 1631. Currently, Method 245.7 

is not specifically mentioned in Table II, 

which was an oversight. 

7. The EPA proposes to specify in 

Table II that sodium thiosulfate is to be 

added to samples to remove oxidants 

(e.g., chlorine) for the Table 1B 

parameter 48 (Phenols) and the Table 1C 

parameters 107 to 111 (Alkylated 

phenols). The EPA also proposes to 

restore footnote 5 in Table II for Table 

1C parameters 23, 30, 44, 49, 53, 77, 80, 

81, 91, 93, and 105 (Phenols), and to 

add Footnote 5 for Table 1C parameters 

112 (Adsorbable Organic Halides) and 

113 (Chlorinated Phenolics), and to 

clarify that the addition of sodium 

thiosulfate is only necessary when 

oxidants are present (e.g., chlorine). 

8. The EPA proposes to add a new 

footnote to Table II under Table Ib and 

apply it to the entry for parameter 50, 

Phosphorus—Total. The new Footnote 

25 addresses the fact that many 

laboratories determine total phosphorus 

using EPA Method 200.7, an ICP/AES 

procedure for metals that is also 

approved for phosphorus. However, as 

laboratories often note, the acid 

specified in Table II to preserve metals 

samples is nitric acid, where Table II 

calls out sulfuric acid for phosphorous. 

In both cases the specified pH is a value 

less than or equal to 2. In addition, 

while Table II allows acidified samples 

to held for 6 months, it only allows 

phosphorus samples to be held for 28 

days. The new Footnote 25 reads: 

‘‘When EPA Method 200.7 or another 

approved ICP/AES method is used to 

determine total phosphorus, sulfuric 

acid may be used to preserve the sample 

to pH ≤ 2, or the acid-preserved sample 

for metals may be used for analysis, and 

the holding time for total phosphorus 

may be extended to 6 months.’’ 

V. Incorporation by Reference 

Currently, hundreds of methods and 

alternate test procedures are 

incorporated by reference within 40 

CFR part 136. In most cases, 40 CFR part 

136 contains multiple approved 

methods for a single parameter (or 

pollutant) and regulated entities often 

have a choice in selecting a method. The 

proposed rule contains VCSB methods 

that are incorporated by reference (see 

section V.B of this preamble). The 

proposed VCSB methods are consistent 

with the requirements of the National 

Technology Transfer and Advancement 

Act (NTTAA), under which Federal 

agencies should use technical standards 

developed or adopted by the VCSBs if 

compliance would not be inconsistent 

with applicable law or otherwise 

impracticable (see section VI of this 

preamble). The proposed copyrighted 

VCSB methods are available on their 

respective websites 

(standardmethods.org and astm.org) to 

everyone at a cost determined by the 

VCSB, generally from $60 to $80. Both 

organizations also offer memberships or 

subscriptions that allow unlimited 

access to their methods. The cost of 

obtaining these methods is not a 

significant financial burden for a 

discharger or environmental laboratory, 

making the methods reasonably 

available. 

This proposal includes EPA Method 

1621, EPA Method 1628, and EPA 

Method 1633A (see section V.A of this 

preamble) and ASTM D8421–24, 

Standard Method ‘‘4500–PAA Peracetic 

Acid (Residual)’’, and Standard Method 

‘‘4500–H2O2 Hydrogen Peroxide 

(Residual)’’ for four parameter types (see 

section V.B of this preamble) which the 

EPA proposes to incorporate by 

reference. The EPA methods and the 

vendor methods are available free of 

charge on their respective websites, 

therefore the EPA methods and vendor 

methods incorporated by reference are 

reasonably available. 

Other standards appear in the 

amendatory text of this document and 

have already been approved for the 

locations in which they appear. 

A. Changes to 40 CFR 136.3 To Include 

Three New EPA Methods and Their 

Associated Parameters 

The EPA proposes to add three new 

EPA methods and their associated 

parameters to 40 CFR 136.3: EPA 

Method 1621: Determination of 

Adsorbable Organic Fluorine (AOF) in 

Aqueous Matrices by Combustion Ion 

Chromatography (CIC), EPA Method 

1628: Polychlorinated Biphenyl (PCB) 

Congeners in Water, Soil, Sediment, 

Biosolids, and Tissue by Low-resolution 

GC/MS using Selected Ion Monitoring, 

and EPA Method 1633A: Analysis of 

Per- and Polyfluoroalkyl Substances 

(PFAS) in Aqueous, Solid, Biosolids, 

and Tissue Samples by LC–MS/MS. All 

three of these methods have multilaboratory validation studies that 

demonstrate they perform well in a 

wide variety of wastewater types at 

multiple laboratories. These methods 

include performance (or quality control) 

criteria that the EPA generated by 

statistically analyzing the data from the 

multi-laboratory validation studies. The 

multi-laboratory validation study 

reports and methods are available to the 

public on the EPA’s Clean Water Act 

Analytical Methods website at https://

www.epa.gov/cwa-methods, and in the 

docket to this proposed rulemaking. 

Adding these methods and parameters 

to 40 CFR part 136 does not require the 

permitting authority to require 

monitoring for those parameters, but it 

informs the permitting authority and 

discharger that there is an available 

method that has been validated and 

tested. Once these methods are finalized 

in 40 CFR part 136, then use of the 

approved test procedure is required if 


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any of these parameters are added to a 

NPDES permit. The EPA proposes to 

add the parameter ‘‘Adsorbable Organic 

Fluorine,’’ (AOF) to Table Ic with the 

approved test procedure EPA Method 

1621. EPA Method 1621 determines 

adsorbable organic fluorine by passing 

an aqueous sample through two 

granular activated carbon columns. The 

columns are rinsed with sodium nitrate 

to remove inorganic fluoride, combusted 

at ≥1000 °C in an oxygen or oxygen/ 

argon stream, and the gaseous hydrogen 

fluoride is absorbed into reagent water. 

The fluoride is separated by ion 

chromatography (IC), identified by 

comparing sample fluoride retention 

time to retention times for calibration 

standards acquired under identical Ic 

conditions, and then quantified using 

the external standard technique. 

The EPA proposes to redesignate all 

tables in 136.3 with a lower case letter, 

for example Table IA would be ‘‘Table 

Ia—List of Approved Biological 

Methods for Wastewater and Sewage 

Sludge.’’ This redesignation of the table 

titles is needed to avoid confusion with 

the currently existing Table II (Roman 

numeral two) and the new table for 

PCBs in order to distinguish between 

Roman numeral one followed by the 

letter ‘‘I’’ and Roman numeral two. Then 

Tables Ii and Ij will be added, as 

discussed below. The number format for 

Table II—Required Containers, 

Preservation Techniques, and Holding 

Times will remain unchanged. 

The EPA proposes to add the 209 

Polychlorinated Biphenyl (PCB) 

Congeners and Total PCBs as new 

parameters in a new Table Ii with the 

approved test procedure EPA Method 

1628. Method 1628 detects all PCB 209 

congeners, which are all the compounds 

that make up the class of chemicals 

called ‘‘PCBs.’’ The new parameter 

called ‘‘Total PCBs’’ will be the 

summation of all the detected PCB 

congeners in the sample as determined 

by Method 1628. The summation will 

use zero (0) for the contribution of the 

congeners that are not detected. 

Otherwise, every method blank would 

have a non-zero result, even when no 

congeners are detected, affecting 

assessments of the sample results 

relative to the method blank. There is no 

method detection limit (MDL) for Total 

PCBs because it is the sum of the results 

for many individual parameters. Method 

blanks and samples with no detects are 

reported as ‘‘ND’’ for non-detect, or a 

similarly appropriate non-numeric 

value. Method 1628 analyzes samples 

by spiking them with isotope dilution 

standards, extracting the PCBs using 

separatory funnel extraction or solidphase extraction, cleaning the extracts 

with a Florisil® column, and analyzing 

the sample extracts using GC/MS with 

selected ion monitoring. Because the 

full names of the PCB congeners are 

long and contain many numbers 

indicating the positions of the chlorine 

substituents (e.g., 2,3,3′,4,4′,5- 

Hexachlorobiphenyl), they are often 

expressed as a ‘‘congener number’’ in 

the format ‘‘PCB–XYZ,’’ where ‘‘XYZ is 

a number between 1 and 209. The EPA 

has included the congener numbers in 

Table Ii to facilitate consistency in 

reporting of the results for these new 

parameters. 

The EPA proposes to add the 40 target 

PFAS analytes in Method 1633A as new 

parameters in a new Table Ij, with the 

approved test procedure EPA Method 

1633A. Method 1633A analyzes samples 

by spiking them with isotope dilution 

standards, subjecting them to solidphase extraction and activated carbon 

cleanup, and analyzing the sample 

extracts using liquid chromatographytandem mass spectrometry (LC–MS/ 

MS). 

The EPA proposes to add these new 

parameters to the relevant section of 

Table II—Required Containers, 

Preservation Techniques, and Holding 

Times. The specifications for the 

containers, preservation techniques, and 

holding times for these parameters are 

the same as the specifications provided 

in the method. 

B. Changes to 40 CFR 136.3 To Include 

New Parameters and Methods Published 

by VCSBs and Vendors 

The EPA solicited VCSBs and relevant 

vendors to submit methods, along with 

study reports and validation data, for 

the following parameters: the PFAS 

parameters listed in Method 1633A, 

peracetic acid, and hydrogen peroxide. 

The VCSBs or vendors submitted data 

that demonstrate that their methods can 

be used at multiple laboratories and can 

reliably detect and quantify the 

parameter in a wide variety of 

wastewater types (as the EPA does with 

its own CWA methods). The methods 

and multi-laboratory study reports for 

each of the following methods are in the 

docket for this rulemaking. The EPA 

proposes to add the following 

parameters and methods to 40 CFR part 

136. 

The EPA also proposes to add these 

new parameters to the relevant section 

of Table II—Required Containers, 

Preservation Techniques, and Holding 

Times. The specifications for the 

containers, preservation techniques, and 

holding times for peracetic acid, and 

hydrogen peroxide are the same as the 

specifications provided in the methods. 

The preservation and holding time 

specifications for the PFAS parameters 

parallel those from EPA Method 1633A. 

1. ‘‘ASTM D8421–24 Standard Test 

Method for Determination of Per- and 

Polyfluoroalkyl Substances (PFAS) in 

Aqueous Matrices by Co-solvation 

followed by Liquid Chromatography 

Tandem Mass Spectrometry (LC/MS/ 

MS),’’ as an approved test procedure for 

the 40 PFAS analytes being added as 

new parameters in Table Ij. ASTM 

D8421–24 analyzes aqueous samples by 

adding labeled surrogates to a 5-mL 

sample in the original container, adding 

5 mL of methanol, filtering the sample, 

adjusting the pH and injecting a small 

aliquot of the extract into an LC–MS/MS 

instrument. 

2. The EPA proposes to add the 

parameter ‘‘Peracetic acid (PAA)’’ to 

Table Ib and approve Standard Method 

‘‘4500–PAA Peracetic Acid (Residual).’’ 

This method uses a simple handheld 

instrument that uses N,N-diethyl–pphenylenediamine (DPD) chemical 

indicator (for PAA) followed by 

colorimetric detection. It is similar to 

the colorimetric methods used for 

residual chlorine. This new parameter 

will provide POTWs and other 

wastewater treatment permittees that 

utilize peracetic acid as an alternative to 

chlorine-based disinfectants with an 

approved method to monitor their 

discharges. 

3. The EPA also proposes to add the 

parameter ‘‘Hydrogen Peroxide (H2O2),’’ 

to Table Ib and approve Standard 

Method ‘‘4500–H2O2 Hydrogen Peroxide 

(Residual).’’ This method uses a simple 

handheld instrument that uses ferric 

thiocyanate chemical indicator (for 

H2O2) followed by colorimetric 

detection. It is similar to the 

colorimetric methods used for residual 

chlorine. Hydrogen peroxide is a byproduct of the use of Peracetic acid as 

an alternative to chlorine-based 

disinfectants and in conjunction with 

the addition of the new parameter 

‘‘Peracetic acid (PAA),’’ Standard 

Method ‘‘4500–H2O2 Hydrogen Peroxide 

(Residual) will provide POTWs and 

other wastewater treatment permittees 

that utilize peracetic acid with approved 

methods to monitor their discharges. 

VI. Statutory and Executive Order 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review Executive Order 

14094: Modernizing Regulatory Review 

This action is not a significant 

regulatory action as defined in 

Executive Order 12866, as amended by 

Executive Order 14094, and was 

therefore not subject to a requirement 

for Executive Order 12866 review. 


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B. Paperwork Reduction Act 

This action does not impose an 

information collection burden under the 

Paperwork Reduction Act. This rule 

does not impose any information 

collection, reporting, or recordkeeping 

requirements. This proposal would 

merely add or revise CWA test 

procedures. 

C. Regulatory Flexibility Act 

I certify that this action would not 

have a significant economic impact on 

a substantial number of small entities 

under the Regulatory Flexibility Act. 

This action would not impose any 

requirements on small entities. This 

action would approve new and revised 

versions of CWA testing procedures. 

Generally, these changes improve data 

quality. In general, the EPA expects the 

proposed revisions would lead to few 

direct costs. Adding these parameters 

and methods to 40 CFR part 136 does 

not require the permitting authority to 

require monitoring that parameter, but it 

informs the permitting authority and 

discharger that there is an available 

method that has been validated and 

tested in a wide variety of wastewater 

types. If a permittee is already 

monitoring for one of more of the 

parameters, then the permittee may 

need to change methods. This would 

not be a significant change in cost, given 

that the permittee is already paying a 

laboratory to analyze for the 

parameter(s). The EPA proposes 

methods that would be incorporated by 

reference. If a permittee elected to use 

these methods, they could incur a small 

cost associated with obtaining these 

methods from the listed sources. See 

section IV of this preamble. 

D. Unfunded Mandates Reform Act 

This action does not contain an 

unfunded mandate as described in the 

Unfunded Mandates Reform Act, 2 

U.S.C. 1531–1538, and does not 

significantly or uniquely affect small 

governments. The action imposes no 

enforceable duty on any state, local or 

tribal governments or the private sector. 

E. Executive Order 13132: Federalism 

This proposed rule does not have 

federalism implications. It would 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. 

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. This rule would 

merely approve new and revised 

versions of test procedures. The EPA 

does not expect the proposal would lead 

to any costs to any tribal governments, 

and if incurred, the EPA projects they 

would be minimal. Thus, Executive 

Order 13175 does not apply to this 

action. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

EPA interprets Executive Order 13045 

as applying only to those regulatory 

actions that concern environmental 

health or safety risks that the EPA has 

reason to believe may 

disproportionately affect children, per 

the definition of ‘‘covered regulatory 

action’’ in section 2–202 of the 

Executive Order. Therefore, this action 

is not subject to Executive Order 13045 

because it does not concern an 

environmental health risk or safety risk. 

Since this action does not concern 

human health, the EPA’s policy on 

Children’s Health also does not apply. 

H. Executive Order 13211: Actions That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This action is not subject to Executive 

Order 13211 because it is not a 

significant regulatory action under 

Executive Order 12866. 

I. National Technology Transfer and 

Advancement Act of 1995 

This action involves technical 

standards. The EPA proposes to approve 

the use of technical standards 

developed and recommended by the 

Standard Methods Committee and 

ASTM International for use in 

compliance monitoring where the EPA 

determined that those standards meet 

the needs of CWA programs. As 

described above, this proposal is 

consistent with the NTTAA. 

J. Executive Order 12898: Federal 

Actions To Address Environmental 

Justice in Minority Populations and 

Low-Income Populations and Executive 

Order 14096: Revitalizing Our Nation’s 

Commitment to Environmental Justice 

for All 

The EPA believes that this type of 

action does not concern human health 

or environmental conditions and 

therefore cannot be evaluated with 

respect to potentially disproportionate 

and adverse effects on communities 

with environmental justice concerns. 

This action has no effect on 

communities because this action will 

approve new CWA testing procedures. 

These changes would provide increased 

flexibility for the regulated community 

in meeting monitoring requirements 

while improving data quality. Adding 

new parameters to 40 CFR part 136 does 

not require the parameters to be 

monitored. In addition, this update to 

the CWA methods will incorporate 

technological advances in analytical 

technology. Although this action does 

not concern human health or 

environmental conditions, the EPA 

identifies and addresses environmental 

justice concerns by identifying and 

addressing, as appropriate, 

disproportionately high and adverse 

human health or environmental effects 

of their programs, policies, and 

activities on minority populations 

(people of color) and low-income 

populations. 

List of Subjects in 40 CFR Part 136 

Environmental protection, 

Incorporation by reference, Reporting 

and recordkeeping requirements, Test 

procedures, Water pollution control. 

Michael S. Regan, 

Administrator. 

For the reasons set forth in the 

preamble, the EPA proposes to amend 

40 CFR part 136 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. Amend § 136.3 by: 

■ a. Redesignating tables IA through IH 

as tables Ia through Ih, respectively; 

■ b. In paragraph (a): 

■ i. Revising the introductory text; 

■ ii. Revising newly redesignated tables 

Ib and Ic; 

■ iii. In newly redesignated table Id, 

revising the third column heading and 

the entry for ‘‘53. Parathion ethyl’’; 

■ iv. Adding in alphabetical order tables 

Ii and Ij; and 

■ c. In paragraph (b): 

■ i. Revising the introductory text; 

■ ii. Redesignating paragraphs (b)(8)(xi) 

through (xvi) as paragraphs (b)(8)(xiv) 

through (xix) and adding new 

paragraphs (b)(8)(xi) through (xiii); 

■ iii. Revising and republishing 

paragraph (b)(10); 


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■ iv. Removing paragraph (b)(13)(i)(A), 

and redesignating paragraphs 

(b)(13)(i)(B) through (X) as paragraphs 

(b)(13)(i)(A) through (W); 

■ v. Adding paragraph (b)(15)(lxxi); 

■ vi. Removing paragraphs (b)(20)(ii) 

through (v), and redesignating 

paragraphs (b)(20)(vi) through (x) as 

paragraphs (b)(ii) through (vi); 

■ vii. Revising paragraph (b)(38)(i); and 

■ viii. Removing paragraph (b)(41). 

■ d. In paragraph (e), table II: 

■ i. Redesignating entries ‘‘Table IA’’ 

through ‘‘Table IH’’ as ‘‘Table Ia’’ 

‘‘through Table Ih’’, respectively; 

■ ii. Revising the entry for ‘‘4. 

Ammonia’’ under Table Ib-Inorganic 

Tests; 

■ iii. Revising entries for ‘‘48. Phenols’’ 

and ‘‘50. Phosphorus, total’’, and adding 

entries for ‘‘77. Hydrogen Peroxide’’ and 

‘‘78. Peracetic Acid’’ under Table Ib— 

Metals; 

■ iv. Revising the table entitled ‘‘Table 

Ic-Organic Tests’’; 

■ v. Adding in alphabetical order 

entries for ‘‘Table Ii—Polychlorinated 

Biphenyl Congener Tests’’ and ‘‘Table 

Ij—Per- and Polyfluorinated Alkyl 

Substances Tests’’; 

■ vi. Revising footnotes 5 and 17 and 

■ vii. Adding footnotes 25 through 29. 

The 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, Ih, Ii, and Ij of this 

section. The methods listed in Tables Ia, 

Ib, Ic, Id, Ie, If, Ig, Ih, Ii, and Ij are 

incorporated by reference, see paragraph 

(b) of this section, with the exception of 

EPA Methods 200.7, 601–613, 624.1, 

625.1, 1613, 1624, and 1625. The full 

texts of Methods 601–613, 624.1, 625.1, 

1613, 1624, and 1625 are printed in 

appendix A of this part, and the full text 

of Method 200.7 is printed in appendix 

C of this part. The full text for 

determining the method detection limit 

when using the test procedures is given 

in appendix B of this part. 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 texts of the 

referenced test procedures are 

incorporated by reference into Tables Ia, 

Ib, Ic, Id, Ie, If, Ig, Ih, Ii, and Ij. The year 

after the method number indicates the 

latest editorial change of the method. 

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, Ih, Ii, and Ij, 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 and 136.5. 

Under certain circumstances (paragraph 

(c) of this section, in § 136.5(a) through 

(d) or 40 CFR 401.13) other additional 

or alternate test procedures may be 

used. 

* * * * * 


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~ OF APPROVED INORGA~IC TEST PROCEDURES 

Standard USGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

1. Acidity, as Electrometric endpoint or 2310 D-2020 D1067-16 1-1020-85 2 

CaCO3, mg/L phenolphthalein endpoint 

2. Alkalinity, as Electrometric or 2320 B-2021 D1067-16 973.43 3, 1-

CaCO3, mg/L Colorimetric titration to 1030-85 2 

pH 4.5, Manual 

Automatic 310.2 1-2030-85 2 

(Rev. 

1974)1 

3. Aluminum- Digestion\ followed by 

Total,4mg/L any of the following: 

AA direct aspiration 32 3111 D- 1-3051-85 2 

2019 or 

3111 E-2019 

AA furnace 3113 B-2020 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Rev4.2 

(2003) 62, 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

Direct Current Plasma D4190-15 See footnote :io 

(DCP) 32 

4. Ammonia (as Manual distillation 6 or 350.1, 4500-NH3B- 973.49 3 

N),mg/L gas diffusion (pH> 11), Rev. 2.0 2021 

followed by any of the (1993) 

following: 

N esslerization D1426-15 (A) 973.49 3, 1-

3520-85 2 

Titration 4500-Nlli C2021 

Electrode 4500-Nlli D1426-15 (B) 

D-2021 or 

E-2021 

Manual phenate, 4500-NH3F- See footnote 55 

salicy late, or other 2021 

substituted phenols in 

Berthelot reaction-based 

methods 

Automated phenate, 350.1 27, 4500-NH3 1-4523-85 2, Isalicylate, or other Rev. 2.0 G-2021 2522-90 74 

substituted phenols in (1993) 4500-NH3 

Berthelot reaction-based 11-2021 

methods 

Automated electrode See footnote.7 

Ton Chromatography D6919-17 
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Standard USGS/AOACJ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Automated gas diffusion, Timberline 

followed by conductivity Ammonia-001 

cell analysis 68 

Automated gas diffusion FIAlab 100 76 

followed by fluorescence 

detector analysis 

5. Antimony- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 

AA furnace 3113 B-2020 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

TCP/AES 32 200.5, 3120 B-2020 D1976-20 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 R-2020 05673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

6. Arsenic-- Digestion 4, followed by 206.5 

Total,4 mg/L any of the following: (Issued 

1978) 1 

AA gaseous hydride 3114 R-2020 02972-15 (R) 1-3062-85 2 

or 

3114 C-2020 

AA furnace 3113 B-2020 D2972-15 (C) 1-4063-98 45 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64 

(1994) 

7. Barium- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 32 3111 D- 1-3084-85 2 

2019 

AA furnace 3113 B-2020 D4382-18 

ICP/AES 32 200.5, 3120 B-2020 1-4471-97 46 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6977 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.231</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

TCP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

DCP 32 See footnote 30 

8. Beryllium- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 3111 D- D3645-15 (A) I-3095-85 2 

2019 or 

3111 E-2019 

AA furnace 3113 B-2020 D3645-15 (B) 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 200.5, 3120 B-2020 Dl976-20 I-4471-97 46 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 05673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

DCP D4190-15 See footnote 30 

9. Biochemical Dissolved Oxygen 5210 B-2016 973.44 3, p. 17 

oxygen demand Depletion 79 9, I- I 578-78 8, 

(BODs), mg/L See footnotes 

10,57 

10. Boron- ICP/AES 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Total,33 mg/L Rev4.2 

(2003) 62 ; 

200.7, 

Rev. 4.4 

(1994) 

TCP/MS 200.8, 3125 B-2020 05673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP D4190-15 See footnote 30 

11. Bromide, Electrode D1246-16 I-1125-85 2 

mg/L 

Ion Chromatography 300.0, 4110 B- D4327-17 993.30 3, IRev2.l 2020, C- 2057-85 73 

(1993) 2020 or Dand 2020 

300.1, 

Rev 1.0 

(1997) 

crnmv 4140 B-2020 D6508-15 

12. Cadmium- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D3557-17 (A 974.27 3,p. 37 

or 3111 C- orB) 9, I-3135-85 2 

2019 or I-3136-85 2 

AA furnace 3113 B-2020 03557-17 (D) I-4138-89 47 
6978 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.232</GPH>

Standard iUSGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 1-1472-85 2 or 

Rev 4.2 1-4471-97 46 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

DCP 32 D4190-15 See footnote 30 

Voltammetry 11 03557-17 (C) 

13. Calcium- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 3111 8- D511-14 (B) 1-3152-85 2 

2019 or 

3111 D2019 

ICP/AES 200.5, 3120 B-2020 1-4471-97 46 

Rev 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP See footnote 30 

Titrimetric (EDT A) 3500-CaB- DSll-14 (A) 

2020 

Ion Chromatography D6919-17 

14. Dissolved Oxygen 5210 B-2016 See 

Carbonaceous Depletion with 79 footnotes .31 • 57 

biochemical nitrification inhibitor 

oxygen demand 

(CBODs), 

mg/IP 

15. Chemical Titrimetric 410.3 5220 B-2011 D1252-06(12) 973.46 3, p. 17 

oxygen demand (Rev. or C-2011 (A) 9, 1-3560-852 

(COD),mg/L 1978) 1 

Spectrophotometric, 410.4, 5220D- D1252-06(12) See footnotes 

manual or automatic Rev. 2.0 2011 (B) l3, 14• 77, 1-3561-

(1993) 85 2 

16. Chloride, Titrimetric: (silver nitrate) 4500-Cl-B- D512-12 (B) 1-1183-85 2 

mg1L 2021 

(Mercuric nitrate) 4500-Cl-c- D512-12 (A) 973.51 3, I2021 1184-85 2 

Colorimetric: manual 1-1187-85 2 

Automated (ferricyanide) 4500-CI-E- T-2187-85 2 

2021 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6979 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.233</GPH>

Standard USGS/A0AO 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Potentiometric Titration 4500-CJ-o2021 

Ion Selective Electrode D512-12 (C) 

Ion Chromatography 300.0, 4110 B-2020 D4327-17 993.30 3, IRev 2.1 or 2057-90 47 

(1993) 4110 C-2020 

and 

300.1, 

Rev 1.0 

(1997) 

CIE/UV 4140 B-2020 D6508-15 

17. Chlorine- Amperometric direct 4500-CI D- D1253-14 

Total residual, 2011 

mg/L 

Amperometric direct (low 4500-Cl Elevel) 2011 

Iodometric direct 4500-ClB2011 

Back titration ether end- 4500-Cl Cpoint 15 2011 

DPD-FAS 4500-Cl F2011 

Spectrophotometric, DPD 4500-Cl G2011 

Electrode See footnote. 16 

17 A. Chlorine- Amperometric direct 4500-ClD- D1253-14 

Free Available, 2011 

mg/L 

DPD-FAS 4500-Cl F2011 

Spectrophotometric, DPD 4500-CI G2011 

18. Chromium 0.45-micron filtration 

VI dissolved, followed by any of the 

mg/L following: 

AA chelation-extraction 3111 C-2019 1-1232-85 2 

Ion Chromatography 218.6, 3500-Cr C- D5257-17 993.23 3 

Rev. 3.3 2020 

(1994) 

Colorimetric (diphenyl- 3500-CrB- D1687-17 (A) 1-1230-85 2 

carbazide) 2020 

19. Digestion 4, followed by 

Chromium- any of the following: 

Total,4mg/L 

AA direct aspiration 32 3111 B-2019 D1687-17 (B) 974.27 3, I3236-85 2 

AA chelation-extraction 3111 C-2019 

AA furnace 3113 B-2020 D1687-17 (C) 1-3233-93 42 

STGFAA 200.9, 

Rev. 2.2 

(1994) 
6980 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.234</GPH>

Standard USGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 

Rev4.2 

(2003) 62, 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 8-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64 I-

(1994) 4472-97 75 

Dcr32 D4190-15 See footnote 30 

20. Cobalt- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 3111 B-2019 D3558-15 (A p. 37 9, 1-3239-

or 3111 C- or 8) 85 2 

2019 

AA furnace 3113 B-2020 D3558-15 (C) 1-4243-89 47 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 200.7, 3120 8-2020 D1976-20 1-4471-97 46 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 8-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64 I-

(1994) 4472-97 75 

DCP D4190-15 See footnote 30 

21. Color, Colorimetric (ADM!) 2120 F-2021 

platinum cobalt 72 

units or 

dominant 

wavelength, 

hue, luminance 

purity 

Platinum cobalt visual 2120 B-2021 1-1250-85 2 

comparison 

Spectrophotometric See footnote 18 

22. Copper- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D1688-17 (A 974.27 3, p. 37 

or or 8) 9, 1-3270-85 2 

3111 C-2019 or T-3271-85 2 

AA furnace 3113 8-2020 D1688-17 (C) 1-4274-89 47 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 8-2020 D1976-20 1-4471-97 46 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6981 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.235</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

lCP/MS 200.8, 3125 R-2020 05673-16 993.14 3, ,_ 

Rev. 5.4 4020-05 64 , ,_ 

(1994) 4472-97 75 

ocp32 D4190-15 See footnote 30 

23. Cyanide Automated UV Kelada-01. 50 

Total, mg/L digestion/distillation and 

Colorimetry 

Segmented Flow 4500-CN-P- D75 l 1-12(17) 

Injection, In-Line 2021 

Ultraviolet Digestion, 

followed by gas diffusion 

amperometry 

Manual distillation with 335.4, 4500-CN-B- D2036- 10-204-00-1-X 

MgCh, followed by any Rev. 1.0 2021 and C- 09(15)(A), 51 

of the following: (1993) 52 2021 D7284-20 

Flow injection, gas D2036-

diffusion amperometry 09(15)(A) 

D7284-20 

Titrimetric 4500-CN D2036- p. 22 9 

D-2021 09(15)(A) 

Spectrophotometric, 4500-CWE- D2036- I-3300-85 2 

manual 2021 09(15)(A) 

Semi-Automated 19 335.4, 4500-CW 10-204-00-1-X 

Rev. 1.0 N-2021 51 , l-4302-85 2 

(1993) 52 

Ion Chromatography D2036-

09(15)(A) 

Ion Selective Electrode 4500-CWF- D2036-

2021 09(1 S)(A) 

24. Cyanide- Cyanide Amenable to 4500-CW D2036-

Available, Chlorination (CATC); G-2021 09(15)(8) 

mg/L Manual distillation with 

MgCh, followed by 

Titrimetric or 

Spectrophotometric 

Cyanide Amenable to 4500-CWP- D751 l-12(17) 

Chlorination (CA TC) by 2021 

difference; Segmented 

Flow Injection, In-Line 

Ultraviolet Digestion, 

followed by gas diffusion 

amperometry81 

Flow injection and ligand 4500-CW D6888-16 OIA-1677-09 

exchange, followed by gas Q-2021 40 

diffusion amperometry 54 

Automated Distillation Kelada-01 50 

and Colorimetry (no UV 

digestion) 

24.A Flow Injection, followed 4500-CWR- 07237-18 (A) OIA-1677-09 

Cyanide-Free, by gas diffusion 2021 40 

mg/L amperometry 

Manual micro-diffusion D4282-15 

and colorimetry 
6982 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.236</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

25. Fluorido-- Manual distillation 6, 4500-F B- D1179-16 (A) 

Total,mg/L followed by any of the 2021 

following: 

Electrode, manual 4500-F-c- D1179-16 (B) 

2021 

Electrode, automated 4500-F-G- I-4327-85 2 

2021 

Colorimetric, (SPADNS) 4500-F-D2021 

Automated complexone 4500-F-E2021 

Ion Chromatography 300.0, 4110 B-2020 D4327-17 993.30 3 

Rev 2.1 or C-2020 

(1993) 

and 

300.l, 

Rev 1.0 

(1997) 

CIE/UV 4140 B-2020 D6508-15 

26.Gold- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 3111 B-2019 

AA furnace 231.2 3113 R-2020 

(Issued 

1978) I 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP See footnote 30 

27. Hardness- Automated colorimetric 130.1 

Total, as (Issued 

CaCOJ, mg/L 1971) I 

Titrimetric (EDTA) 2340 C-2021 01126-17 973.5213 3, I1338-85 2 

Ca plus Mg as their 2340 B-2021 

carbonates, by any 

approved method for Ca 

and Mg (See Parameters 

13 and 33 ), provided that 

the sum of the lowest 

point of quantitation for 

Ca and Mg is below the 

NPDES pennit 

requirement for Hardness. 

28. Hydrogen Electrometric 4500-WB- D1293-18 (A 973.41 3,Iion(pH), pH measurement 2021 orB) 1586-85 2 

units 

Automated electrode 150.2 Sec footnote 

(Dec. 20 

' 1982) 1 1-2587-85 2 

29. Iridium- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 3111 B-2019 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6983 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.237</GPH>

Standard USGS/AOACJ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

AA furnace 235.2 

(Issued 

1978) 1 

ICP/MS 3125 B-2020 

30. Iron- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D1068-15 (A) 974.27 3,1-

or 3381-85 2 

3111 C-2019 

AA furnace 3113 B-2020 D1068-15 (B) 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

TCP/AES 32 200.5, 3120 B-2020 D1976-20 T-4471-97 46 

Rev.4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 R-2020 05673-16 993.14 3 

Rev. 5.4 

(1994) 

ocp32 D4190-15 See footnote 30 

31. Kjeldahl Manual digestion 19 and 4500-Norg B- D3590-17 (A) 1-4515-91 41 

Nitrogen 5 - distillation or gas 2021 or CTotal, (as N), diffusion, followed by any 2021 and 

mg/L of the following: 4500-NH3 B2021 

Titration 4500-NH3C- 973.48 3 

2021 

Nesslerization D1426-15 (A) 

Electrode 4500-NH3 01426-15 (R) 

D-2021 or 

E-2021 

Semi-automated phenate 350.1, 4500-NH3 

Rev. 2.0 G-2021 or 

(1993) 4500-NH3 

H-2021 

Manual phenate, 4500-NH3F- See footnote 55 

salicylate, or other 2021 

substituted phenols in 

Berthelot reaction-based 

methods 

Automated gas diffusion, Timberline 

followed by conductivity Ammonia-001 

cell analysis 68 

Automated gas diffusion fIAlab 100 76 

followed by fluorescence 

detector analysis 

Automated Methods for TKN that do not require manual distillation 
6984 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.238</GPH>

Standard USGS/AOACJ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Automated phenate, 351.1 1-4551-78 8 

salicylate, or other (Rev. 

substituted phenols in 1978)1 

Berthelot reaction-based 

methods colorimetric 

(auto digestion and 

distillation) 

Semi-automated block 351.2, 4500-NorgD- D359O-17 (B) 1-4515-91 41 

digestor colorimetric Rev.2.O 2021 

( distillation not required) (1993) 

Block digester, followed See footnote 35 

by Auto distillation and 

Titration 

Block digester, followed See footnote 36 

by Auto distillation and 

N csslcrization 

Block Digester, followed See footnote 37 

by Flow injection gas 

diffusion (distillation not 

required) 

Digestion with Hach 10242 70 

peroxydisulfate, followed 

by Spectrophotometric 

(2,6-dimethylphenol) 

Digestion with persulfate, NCASI TNTP 

followed by Colorimetric W109OO 71 

32. Lead- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D3559-15 (A 974.27 3, Ior or B) 3399-85 2 

3111 C-2O19 

AA furnace 3113 B-2020 D3559-15 (D) 1-4403-89 47 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-2O 1-4471-97 46 

Rev.4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

TCP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

DCP32 D419O-15 See footnote 30 

Voltammetry 11 D3559-15 (C) 

33. Digestion 4, followed by 

Magnesium- any of the following: 

Total,4mg/L 

AA direct aspiration 3111 B-2019 D511-14 (B) 974.27 3, I3447-85 2 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6985 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.239</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

ICP/AES 200.5, 3120 B-2020 Dl976-20 I-4471-97 46 

Rev. 4.2 

(2003) 62 ; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 R-2020 05673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP See footnote 30 

Ion Chromatography D6919-17 

34. Digestion4, followed by 

Manganese- any of the following: 

Total,4 mg/L 

AA direct aspiration 32 3111 B-2019 D858-17 (A or 974.27 3, Ior 3111 C- 8) 3454-85 2 

2019 

AA furnace 3113 B-2020 D858-17 (C) 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Rev. 4.2 

(2003) 62 ; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3,IRev. 5.4 4472-97 75 

(1994) 

DCP 32 D4190-15 See footnote 30 

35. Mercury- Cold vapor, Manual 245.1, 3112 B-2020 D3223-17 977.22 3, ITotal,mg/L Rev. 3.0 3462-85 2 

(1994) 

Cold vapor, Automated 245.2 

(Issued 

1974)1 

Cold vapor atomic 245.7 I-4464-01 65 

fluorescence spectrometry Rev. 2.0 

(CVAFS) (2005) 17 

Purge and Trap CV AFS 163 IE 39 

36. Digestion 4, followed by 

Molybdenum- any of the following: 

Total,4mg/L 

AA direct aspiration 3111 D- 1-3490-85 2 

2019 

AA furnace 3 I 13 B-2020 1-3492-96 43 

ICP/AES 200.7, 3120 B-2020 D1976-20 1-4471-97 46 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 8-2020 05673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 
6986 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.240</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

DCP See footnote 30 

37. Nickel- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D1886-14 (A 1-3499-85 2 

or orB) 

3111 C-2O19 

AA furnace 3113 B-2020 D1886-14 (C) 1-4503-89 47 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-2O 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64, I-

(1994) 4472-97 75 

DCP 32 D419O-15 See footnote 30 

38. Nitrate (as Ion Chromatography 300.0, 41 IO B-2020 D4327-17 993.30 3 

N), mg/L Rev. 2.1 or C-2O2O 

(1993) 

and 

300.1, 

Rev. 1.0 

(1997) 

CIE/UV 4140 B-2020 D65O8-15 

Ion Selective Electrode 45OO-N03-

D-2O19 

Colorimetric (Brucine 352.1 973.50 3,419D 

sulfate) (Issued so, p. 28 9 

1971)1 

Spectrophotometric (2,6- Hach 10206 69 

dimethylphenol) 

Nitrate-nitrite N minus 

Nitrite N (See parameters 

39 and 40) 

39. Nitrate- Cadmium reduction, 45OO-N03- D3867-16 (B) 

nitrite (as N), Manual E-2O19 

mg/L 

Cadmium reduction, 353.2, 45OO-N03- D3867-16 (A) 1-2545-90 47 

Automated Rev. 2.0 F-2O19 or 

(1993) 45OO-N03-

1-2019 

Automated hydrazine 45OO-N03-

H-2O19 

Reduction/Colorimetric See footnote 56 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6987 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.241</GPH>

Standard USGS/AOACJ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Ion Chromatography 300.0, 4110 B-2020 D4327-17 993.30 3 

Rev. 2.1 orC-2020 

(1993) 

and 

300.1, 

Rev. 1.0 

(1997) 

CIE/UV 4140 B-2020 D6508-15 

Enzymatic reduction, D7781-14 1-2547-11 66 

followed by automated 1-2548-11 66 

co lo rim etric N07-0003 67 

determination 

Enzymatic reduction, 4500-NO3-

followed by manual J-2018 

co lo rim etric 

determination 

Spec.1rophotometric (2,6- Hach 10206 69 

dimethylphenol) 

40. Nitrite (as Spectrophotometric: 4500-NO2- See footnote 22 

N), mg/L Manual B-2021 

Automated 1-4540-85 2, 

(Diazotization) See footnote 56 

1-2540-90 74 

Automated (*bypass 353.2, 4500-NO3- D3867-16 (A) T-4545-85 2 

cadmium reduction) Rev.2.0 F-2019 

(1993) 4500-NO3 

1-2019 

Manual (*bypass 4500-NO3- D3867-16 (B) 

cadmium or enzymatic E-2019, 

reduction) 4500-NO3-

J-2018 

Ion Chromatography 300.0, 4110 B-2020 D4327-17 993.30 3 

Rev. 2.1 orC-2020 

(1993) 

and 

300.1, 

Rev. 1.0 

(1997) 

CIE/UV 4140 B-2020 D6508-15 

Automated (*bypass D7781-14 1-2547-11 66 

Enzymatic reduction) 1-2548-11 66 

N07-0003 67 

41. Oil and Hexane extractable 1664 5520 B or 

grease-Total material (HEM): n- Rev. B 38 G-2021 34 

recoverable, Hexane extraction and 

mg/L gravimetry 

Silica gel treated I IEM 1664 5520 B or 

(SGT-HEM): Silica gel Rev. B 38 G-2021 34 

treatment and gravimetry and 5520 F2021 34 

42. Organic Combustion 5310 B-2014 D7573-18ael 973.47 3, P- 14 

carbon-Total 21 

(TOC),mg/L 
6988 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.242</GPH>

Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Heated persulfate or UV 5310 C-2014 D4839-03(17) 973.47\ p. 14 

persulfate oxidation 5310 D- 21 

2011 

43. Organic Total Kjeldahl N 

nitrogen (as N), (Parameter 31) minus 

mg/L ammonia N (Parameter 4) 

44. Ortho- Ascorbic acid method: 

phosphate (as 

P), mg/L 

Automated 365.1, 4500-P F- 973.56 3, IRev. 2.0 2021 or G- 4601-85 2, I-

(1993) 2021 2601-90 74 

Manual, single-reagent 4500-P E- D515-88 (A) 973.55 3 

2021 

Manual, two-reagent 365.3 

(Issued 

1978) I 

Ion Chromatography 300.0, 4110 8-2020 D4327-17 993.30 3 

Rev. 2.1 or C-2020 

( 1993) 

and 

300.1, 

Rev. 1.0 

(1997) 

CIE/UV 4140 B-2020 D6508-15 

45. Osmium- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiration 3111 D2019 

AA furnace 252.2 

(Issued 

1978) I 

46. Oxygen, Winkler (Azide 4500-0 (8- D888-18 (A) 973.458 3, 

Dissolved, modification) F)-2021 I-1575-78 8 

mg/L 

Electrode 4500-0 G- D888-18 (B) I-1576-78 8 

2021 

Luminescence-Based 4500-0 H- D888-18 (C) See footnotes 

Sensor 2021 57 58 

' 

47. Digestion 4, followed by 

Palladium- any of the following: 

Total,4mg/L 

AA direct aspiration 31118-2019 

AA furnace 253.2 

(Issued 

1978) I 

ICP/MS 3125 8-2020 

DCP See footnote 30 

48. Phenols, Manual distillation 23, 420.1 5530 8-2021 D1783-01(12) 

mg/L followed by any of the (Rev. 

following: 1978) I 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6989 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.243</GPH>

Standard USGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Colorimetric (4AAP) 420.1 5530 D- D1783-01(12) 

manual (Rev. 2021 24 (A or B) 

1978) l 

Automated colorimetric 420.4 

(4AAP) Rev. 1.0 

(1993) 

49. Phosphorus Gas-liquid See footnote 25 

(elemental), chromatography 

mg/L 

50. Digestion 19, followed by 4500-P B 973.55 3 

Phosphorus- any of the following: (5)-2021 

Total, mg/L 

Manual 365.3 4500-P E- D515-88 (A) 

(Issued 2021 

1978) 1 

Automated ascorbic acid 365.1 4500-P (F- 973.56 3, Ireduction Rev. 2.0 H)-2021 4600-85 2 

(1993) 

ICP/AES 4• 32 200.7, 3120 B-2020 I-4471-97 46 

Rev. 4.4 

(1994) 

Semi-automated block 365.4 D515-88 (B) 1-4610-91 44 

digestor (TKP digestion) (Issued 

1974) I 

Digestion with persulfate, NCASITNTP 

followed by Colorimetric W10900 71 

S 1. Platinum- Digestion 4, followed by 

Total,4 mg/L any of the following: 

AA direct aspiralion 3111 B-2019 

AA furnace 255.2 

(Issued 

1978) I 

ICP/MS 3125 D-2020 

DCP See footnote 30 

52. Digestion 4, followed by 

Potassium- any of the following: 

Total,4 mg/L 

AA direct aspiration 3111 B-2019 973.53 3, I3630-85 2 

ICP/AES 200.7, 3120 B-2020 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

Flame photometric 3500-KD2020 

Electrode 3500-K C2020 

Ion Chromatography D6919-17 

53. Residue- Gravimetric, 103-105° 2540 B-2020 I-3750-85 2 

Total, mg/L 
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Standard USGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

54. Residue- Gravimetric, 180° 2540 C-2020 D5907-18 (B) 1-1750-85 2 

Filterable, mg/L 

55. Residue- Gravimetric, 103-105° 2540 D- D5907-18 (A) 1-3765-85 2 

Non-filterable post-washing of residue 2020 

(TSS), mg/L 

56. Residue- Volumetric (Imhoff cone), 2540 F-2020 

Settleable, or gravimetric 

mg/L 

57. Residue- Gravimetric, 550° 160.4 2540 E-2020 1-3753-85 2 

Volatile, mg/L (Issued 

1971) 1 

58. Rhodium- Digestion 4, followed by 

Total, 4 mg/L any of the following: 

AA direct aspiration, or 3111 B-2019 

AA furnace 265.2 

(Issued 

1978) 1 

ICP/MS 3125 B-2020 

59. Digestion 4, followed by 

Ruthenium- any of the following: 

Total,4mg/L 

AA direct aspiration, or 3111 B-2019 

AA furnace 267.2 I 

ICP/MS 3125 B-2020 

60. Selenium- Digestion 4, followed by 

Total, 4 mg/I, any of the following: 

AA furnace 3113 R-2020 03859-15 (R) 1-4668-98 45 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 

Rev4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 [05673-16 993.14 3, IRev. 5.4 4020-05 64 1-

(1994) 4472-97 75 

AA gaseous hydride 3114 B- ID3859-15 (A) 1-3667-85 2 

2020,or 

3114 C-2020 

61. Silica- 0.45-micron filtration 

Dissolved, 33 followed by any of the 

mg/L following: 

Colorimetric, Manual 4500-SiO2 D859-16 1-1700-85 2 

C-2021 

Automated 4500-SiO2 1-2700-85 2 

(Molybdosilicate) E-2021 or F2021 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6991 


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Standard USGS/AOACJ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

ICP/AES 200.5, 3120 B-2020 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

62. Silver- Digestion 4, 26, followed 

TotaJ,4,28 mg/L by any of the following: 

AA direct aspiration 3111 B-2019 974.27 3, p. 37 

or 9, 1-3720-85 2 

3111 C-2019 

AA furnace 3113 B-2020 1-4724-89 ~7 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

TCP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4472-97 75 

(1994) 

DCP See footnote 30 

63. Sodium- Digestion 4, followed by 

Total,4mg/L any ofthc following: 

AA direct aspiration 3111 B-2019 973.54 3, I3735-85 2 

ICP/AES 200.5, 3120 B-2020 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP Sec footnote 30 

Flame photometric 3500-NaB2020 

Ion Chromatography D6919-17 

64. Specific Wheatstone bridge 120.1 2510 B-2021 D1125-95(99) 973.40 3, Iconductance, (Rev. (A) 2781-85 2 

micromhos/cm 1982) 1 

at25 8C 

65. Sulfate (as Automated colorimetric 375.2, 4500-SO/-

SO4), mg/L Rev.2.0 F-2021 or 

(1993) G-2021 
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Standard USGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

Gravimetric 4500-SOi· 925.54 3 

C-2021 or 

D-2021 

Turbidimetric 4500-SOi· D516-16 

E-2021 

Ion Chromatography 300.0, 4110 B-2020 D4327-17 993.303, IRev. 2.1 orC-2020 4020-05 64 

(1993) 

and 

300.1, 

Rev. 1.0 

(1997) 

CIE/UV 4140 B-2020 ID6508-15 

66. Sulfide (as Sample Pretreatment 4500-s2-B, 

S),mg/L C-2021 

Titrimetric (iodine) 4500-s2-F- 1-3840-85 2 

2021 

Colorimetric (methylene 4500-S2 Dblue) 2021 

Ion Selective Electrode 4500-s2-o- [04658-15 

2021 

67. Sulfite (as Tilrimelric (iodine-iodate) 4500-SoiSO3), mg/L B-2021 

68. Surfactants, Colorimetric (methylene 5540 C-2021 [D2330-20 

mg/L blue) 

69. Thermometric 2550 B-2010 See footnote 29 

Temperature, 0 

C 

70. Thallium- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 3111 B-2019 

AA furnace 279.2 3113 B-2020 

(Issued 

1978) I 

STGFAA 200.9, 

Rev. 2.2 

(1994) 

ICP/AES 200.7, 3120 B-2020 [01976-20 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 ID5673-I6 993.14 3, IRev. 5.4 4471-97 46 I-

(1994) 4472-97 75 

71. Tin- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 3111 B-2019 T-3850-78 8 

AA furnace 3113 B-2020 

STGFAA 200.9, 

Rev. 2.2 

(1994) 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6993 


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Standard USGS/AOAC/ 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

ICP/AES 200.5, 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993. 14 3 

Rev. 5.4 

(1994) 

72. Titanium- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 3111 D2019 

AA furnace 283.2 

(Issued 

1978) I 

ICP/AES 200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3 

Rev. 5.4 

(1994) 

DCP See footnote 30 

73. Turbidity, INephelometric 180.1, 2130 B-2020 D1889-00 1-3860-85 2 

NTU 49 Rev.2.0 See footnotes 

(1993) 59, 60, 61 

74. Digestion 4, followed by 

Vanadium- any of the following: 

Total,4mg/L 

IAA direct aspiration 3111 D2019 

lAA furnace 3113 B-2020 D3373-17 

ICP/AES 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64 

(1994) 

DCP D4190-15 See footnote 30 

75. Zinc- Digestion 4, followed by 

Total,4mg/L any of the following: 

AA direct aspiration 32 3111 B-2019 D1691-17 (A 974.27 3, p. 37 

or 3111 C- or 8) 9, 1-3900-85 2 

2019 

AA furnace 289.2 

(Issued 

1978) 1 
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Standard lJSGS/AOACi 

Parameter Methodology 53 EPA 48 Methods 78 ASTM Other 

ICP/AES 32 200.5, 3120 B-2020 D1976-20 1-4471-97 46 

Rev. 4.2 

(2003) 62; 

200.7, 

Rev. 4.4 

(1994) 

ICP/MS 200.8, 3125 B-2020 D5673-16 993.14 3, IRev. 5.4 4020-05 64, I-

(1994) 4472-97 75 

ncp32 D4190-15 See footnote 30 

76. Acid Mine 1627 63 

Drainage 

77. Hydrogen Spectrophotometric, 4500-H2O2 

Peroxide, mg/L Ferric Thiocyanate B-2020 

78. Peracetic Spectrophotometric, DPD 4500-PAA 

Acid, mg/L B-2019 

Table lb Notes: 

1 Methods for Chemical Analysis of Water and Wastes, EP A-600/4-79-020. Revised March 1983 and 1979, 

where applicable. U.S. EPA. 

2 Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of WaterResource Investigations of the U.S. Geological Survey, Book 5, Chapter A 1., unless otherwise stated. 1989. 

USGS. 

3 Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, 

Sixteenlh Edition, 4th Revision, 1998. AOAC International. 

1 For the determination of total metals (which are equivalent to total recoverable metals) the sample is not 

filtered before processing. A digestion procedure is required to solubilize analytes in suspended material 

and to break down organic-metal complexes . For non-platform graphite furnace atomic absorption 

determinations, a digestion using nitric acid (as specified in Section 4.1.3 of Methods for 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 (FLAA) determinations, a combination acid (nitric and hydrochloric acids) digestion is 

preferred, prior lo analysis. The approved total recoverable digestion is described as Melhod 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, and200.9 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, 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6995 


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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 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 

lb of this section); 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 effiuent 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 (for a total of36 samples, assuming 9 matrices). If 

results are comparable, the laboratory may dispense with the distillation step for future analysis. 

Comparable is defined as< 20% RPD for all tested matrices). Alternatively, the two populations of spike 

recovery percentages may be compared using a recognized statistical test. 

7 Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto 

Analyzer II. February 19, 1976. Bran & Luebbe Analyzing Technologies Inc. 

8 The approved method is that cited in Methods for Determination of Inorganic Substances in Water and 

Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, 

Chapter Al. 1979. USGS. 

9 American National Standard on Photographic Processing Effiuents. April 2, 1975. American National 

Standards Institute. 

10 In-Situ Method I 003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 

2009. In-Situ Incorporated. 

11 The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is 

acceptable. 

12 Carbonaceous biochemical oxygen demand (CBODs) must not be confused with the traditional BODs 
6996 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


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test method which measures "total 5-day BOD." The addition of the nitrification inhibitor is not a 

procedural option but must be included to report the CBODs parameter. A discharger whose permit requires 

reporting the traditional 8005 may not use a nitrification inhibitor in the procedure for reporting the results. 

Only when a discharger's permit specifically states CBOD5 is required can the permittee report data using a 

nitrification inhibitor. 

13 OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation. 

14 Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company. 

15 The back-titration method will be used to resolve controversy. 

16 Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research 

Incorporated. The calibration graph for the Orion residual chlorine method must be derived using a reagent 

blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/I 00 mL 

solution, respectively. 

17 Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-

001. Revision 2.0, February 2005. US EPA. 

18 National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 253 

(1971) and Technical Bulletin 803, May 2000. 

19 When using a method with block digestion, this treatment is not required. 

20 Industrial Method NU111ber 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & 

Luebbe {Technicon) Autoanalyzer II. October 1976. Bran & Luebbe Analyzing Technologies. 

21 Methods for Analysis of Organic Substances in Water and Fluvial Sediments, Techniques ofWaterResources Investigations of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised 1987). 1987. 

USGS. 

22 Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. 

Hach Company. 

23 Just prior to distillation, adjust the sulfuric-acid-preserved sample to pl I 4 with I I 9 NaOI I. 

24 The colorimetric reaction must be conducted at a pH of 10.0 ± 0.2. 

25 Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid 

Chromatography, Juurnal o[Chromatography, 47(3):421-426. 

26 Approved methods for the analysis of silver in industrial wastewaters at concentrntions of 1 rng/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 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6997 


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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 of2 M Na2S2O3 and NaOH. Standards 

should be prepared in the same manner. For levels of silver below 1 mg/I, the approved method is 

satisfactory. 

27 The use of EDT A 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. 

28 For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen 

iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by 

adding 4.0 mL of concentrated NH4OH, 6.5 g ofKCN, and 5.0 mL ofa 1.0 N solution of[z 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 l mL of the cyanogen iodide solution and let stand 

1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water. 

29 "Water Temperature-fufluential Factors, Field Measurement and Data Presentation," Techniques of 

Water-Resources fuvestigations of the U.S. Geological Survey, Book 1, Chapter Dl. 1975. USGS. 

30 Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace 

Elemental Analysis of Water and Wastes. 1986-Revised 1991. Thermo Jarrell Ash Corporation. 

31 In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by 

Optical Probe. 2009. In-Situ Incorporated. 

32 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. 

Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. 

CEM Corporation. 

33 When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from 

start until completion of analysis. 

34 Only use n-hexane (n-Hexane-85% minimum purity, 99.0% min. saturated C6 isomers, residue less 

than 1 mg/L) extraction solvent when determining Oil and Grease parameters-Hexane Extractable 

Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). 

Use of other extraction solvents is prohibited. 
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35 Method PAl-DK0l, Nitrogen, Total Kje1dah1, Block Digestion, Steam DistiUation, Titrimetric 

Detection. Revised December 22, 1994. OI Analytical. 

36 Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric 

Detection. Revised December 22, 1994. OJ Analytical. 

37 Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised 

December 22, 1994. 01 Analytical. 

38 Method 1664 Rev. B, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated nHexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry, EPA-821-

R-10-001, February 2010, U.S. EPA. 

39 Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic 

Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August 2002, U.S. EPA. The application of 

clean techniques described in EPA's Method 1669: Sampling Ambient Water for Trace Metals at EPA 

Water Quality Criteria Levels, EPA-821-R-96-011, are recommended to preclude contamination at lowlevel, trace metal determinations. 

40 Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 

2010. 01 Analytical. 

41 Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an 

Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS. 

42 Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Chromium in Water by Graphite Furnace Atomic Absorption 

Spectrophotometry. 1993. USGS. 

43 Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 

1997. USGS. 

44 Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated 

Colorimetric Finish That Includes Dialysis. 1992. USGS. 

45 Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic 

Absorption Spectrometry. 1999. USGS. 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 6999 


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46 Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Elements in Whole-water Digests Using Inductively Coupled PlasmaOptical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS. 

47 Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality 

Laboratory-Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. 

USGS. 

48 Unless otherwise indicated, all EPA methods, excluding EPA Method300.1, are published in U.S. EPA. 

May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, 

EP A/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in 

Environmental Samples, EPA/600/R-93/100. EPA Method 300.l is U.S. EPA. Revision 1.0, 1997, 

including errata cover sheet April 27, 1999. Determination oflnorganic Ions in Drinking Water by Ion 

Chromatography. 

49 Styrene divinyl benzene beads (e.g., AMCO-AEPA-1 or equivalent) and stabilized formazin (e.g., Hach 

StablCalTM or equivalent) are acceptable substitutes for formazin. 

5° Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and 

Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001. US EPA. Note: A 450-WUV lamp may be 

used in this method instead of the 550-W lamp specified ifit 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. 

51 Quik.Chem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and 

Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis. Revision 

2.2, March 2005. Lachat Instruments. 

52 When using sulfide removal test procedures described in EPA Method 335.4, reconstitute particulate 

that is filtered with the sample prior to distillation. 

53 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. 

54 Samples analyzed for available cyanide using OJ Analytical method OIA-1677-09 or ASTM method 

D6888-l6 that contain particulate matter may be filtered prior to the ligand exchange reagents have been 

added to the samples. 

55 Analysts should be aware that pH optima and chromophore absorption maxima might differ when 
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phenol is replaced by a substituted phenol as the color reagent in Berthelot Reaction ("phenolhypochloritc reaction") colorimetric ammonium determination methods. For example, when phenol is 

used as the color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 

nm, respectively-see, Patton, C.J. and S.R. Crouch. March 1977. Anal. Chem. 49:464-469. These 

reaction parameters increase to pH> 12.6 and 665 nm when salicylate is used as the color reagent-see, 

Krom, M.D. April 1980. The Analyst 105:305-316. 

56 Easy (I-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla. 

57 Hach Method I 0360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and 

for Use in the Determination of BOD5 and CBOD5. Revision 1.2, October 2011. Hach Company. This 

method may be used to measure dissolved oxygen when performing the methods approved in Table lb of 

this section for measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical 

oxygen demand (CBOD). 

58 In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Mca'>urcmcnt by Optical Probe. 2009. In-Situ 

Incorporated. 

59 Mitchell Method M533 l, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. 

Leck Mitchell. 

60 Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. 

Leck Mitchell. 

61 Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. 

Thermo Scientific. 

62 EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed 

Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/600/R-06/115. Revision 4.2, October 

2003. US EPA. 

63 Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. 

December 2011. US EPA. 

64 Techniques and Methods Book 5-Bl, Determination of Elements in Natural-Water, Biota, Sediment and 

Soil Samples Using Collision/Reaction Cell Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, 

Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis, 2006. USGS. 

65 Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey 

National Water Quality Laboratory-Determination of Organic Plus Inorganic Mercury in Filtered and 

Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS. 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7001 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.255</GPH>

66 USGS Techniques and Methods 5-B8, Chapter 8, Section B, Methods of the National Water Quality 

Laboratory Book 5, Laboratory Analysis, 2011 USGS. 

67 NECi Method N07-0003, "Nitrate Reductase Nitrate-Nitrogen Analysis," Revision 9.0, March 2014, 

The Nitrate Elimination Co., Inc. 

68 Timberline Instruments, LLC Method Ammonia-001, "Determination of Inorganic Ammonia by 

Continuous Flow Gas Diffusion and Conductivity Cell Analysis," June 2011, Timberline Instruments, 

LLC. 

69 Hach Company Method 10206, "Spectrophotometric Measurement ofNitrate in Water and 

Wastewater," Revision 2.1, January 2013, Hach Company. 

70 Hach Company Method l 0242, "Simplified Spectrophotometric Measurement of Total Kjeldahl 

Nitrogen in Water and Wastewater," Revision 1.1, January 2013, Hach Company. 

71 National Council for Air and Stream Improvement (NCASI) Method TNTP-W10900, "Total (Kjeldahl) 

Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate 

Digestion," June 2011, National Council for Air and Stream Improvement, Inc. 

72 The pH adjusted sample is to be adjusted to 7.6 for NPDES reporting purposes. 

73 1-2057-85 U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. 

Al 1989, Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, 1989. 

74Methods 1-2522-90, 1-2540-90, and 1-2601-90 U.S. Geological Survey Open-File Report 93-125, 

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of 

Inorganic and Organic Constituents in Water and Fluvial Sediments, 1993. 

75 Method 1-1472-97, U.S. Geological Survey Open-File Report 98-165, Methods of Analysis by the U.S. 

Geological Survey National Water Quality Laboratory-Determination of Inorganic and Organic 

Constituents in Water and Fluvial Sediments, 1998. 

76 fIAlab Instruments, Inc. Method fIAlab 100, "Determination of Inorganic Ammonia by Continuous 

Flow Gas Diffusion and Fluorescence Detector Analysis", April 4, 2018, FIAlab Instruments, Inc. 

77 MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR® COD LR/ HR, 

"Spectrophotometric Measurement of Chemical Oxygen Demand in Water and Wastewater", Revision 

1.5, May 2018, MACHEREY-NAGEL GmbH and Co. KG. 

78 Please refer to the following applicable Quality Control Sections: Part 2000 Methods, Physical and 

Aggregate Properties 2020 (2021); Part 3000 Methods, Metals, 3020 (2021); Part 4000 Methods, 

Inorganic Nonmetallic Constituents, 4020 (2022); Part 5000 Methods, and Aggregate Organic 
7002 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.256</GPH>

Constituents, 5020 (2022). These Quality Control Standards are available for download at 

www.standardmethods.org at no charge. 

79 Each laboratory may establish its own control limits by performing at least 25 glucose-glutamic acid 

(GGA) checks over several weeks or months and calculating the mean and standard deviation. The 

laboratory may then use the mean + 3 standard deviations as the control limit for future GGA checks. 

However, GGA acceptance criteria can be no wider than 198 ± 30.5 mg/L for BOD~. GGA acceptance 

criteria for CBOD must be either 198 ± 30.5 mg/L, or the lab may develop control charts under the 

following conditions: dissolved oxygen uptake from the seed contribution is between 0.6 - 1.0 mg/L; 

control charts are performed on at least 25 GGA checks with three standard deviations from the derived 

mean; the RSD must not exceed 7.5%; and any single GGA value cannot be less than 150 mg/L or higher 

than 250 mg/L. 

80 The approved method is that cited in Standard Methods for the Examination of 

Water and Wastewater, 14th Edition, 1976. 

81 Prior to in-line UV digestion followed by gas diffusion amperometry, the sample must be treated as 

specified in SM 4500-CN- P-2021 (4a, b, and c) or ASTM D2036-09(15) (B, steps 21.1.1 through 21.1.5) 

lllillllllll OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE Organic COMPOlNDS 

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

1. Acenaphthene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

2. Acenaphthylene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7003 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.257</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

3. Acrolein GC 603 

GC/MS 624.l 4, 

1624B 

4. Acrylonitrilc GC 603 

GC/MS 624.l 4, 0-4127-96 12 

16248 

5. Anthracene GC 610 

GC/MS 625.1, 6410 8- See footnote 8 p. 

16258 2020 27 

HPLC 610 6440 8- D4657-

2021 92 (98) 

6. Benzene GC 602 6200 C2020 

GC/MS 624.l, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

7. Benzidine Spectro- See footnote 3 p. l 

photometri 

C 

GC/MS 625.1 5, 6410 8-

16258 2020 

HPLC 605 

8. Benzo(a)anthracene GC 610 

GC/MS 625.l, 6410 B- See footnote 8 p. 

16258 2020 27 

HPLC 610 6440 B- 04657-

2021 92 (98) 
7004 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.258</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

9. Benzo(a)pyrene GC 610 

GC!MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

10. GC 610 

8enzo(b )fluoranthene 

GC/MS 625.1, 6410 8- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

11. GC 610 

Benzo(g,h,i)pery lene 

GCIMS 625.1, 6410 B- See footnote 8 p. 

16258 2020 27 

HPLC 610 6440 8- D4657-

2021 92 (98) 

12. GC 610 

8enzo(k)tluoranthene 

GC/MS 625.1, 64108- See footnote 8 p. 

16258 2020 27 

HPLC 610 6440 8- D4657-

2021 92 (98) 

13. 8enzy1 chloride GC See footnote 3 p. 

130 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7005 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.259</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS See footnote 6 p. 

S102 

14. Butyl benzyl GC 606 

phthalate 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625B 2020 27 

15. bis(2- GC 611 

Chloroelhoxy) 

methane 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

16. bis(2-Chloroethyl) GC 611 

ether 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625B 2020 27 

17. bis(2-Ethylhexyl) GC 606 

phthalate 

GC/MS 625.1, 6410B- See footnote 8 p. 

16258 2020 27 

18. GC 601 6200 CBromodichloromethan 2020 

e 

GC/MS 624.1, 6200 Il- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

19. Bromoform GC 601 6200 C2020 
7006 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.260</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS 624.l, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

20. Bromomethane GC 601 6200 C2020 

GC/MS 624.1, 6200 R- 0-4127-96 12, 0-

16248 2020 4436-16 13 

21. 4-8romophenyl GC 611 

phenyl ether 

GC/MS 625.l, 6410 B- See footnote 8 p. 

1625B 2020 27 

22. Carbon GC 601 6200 C- See footnote 3 p. 

tetrachloride 2020 130 

GC/MS 624.l, 6200 B- 0-4127-96 12, 0-

16248 2020 4436-16 13 

23. 4-Chloro-3-methyl GC 604 6420 8-

phenol 2021 

GC/MS 625.1, 64108- See footnote 8 p. 

16258 2020 27 

24. Chlorobenzene GC 601,602 6200 C- See footnote 3 p. 

2020 130. 

GC/MS 624.1, 6200 8- 0-4127-96 12 0-

162413 2020 4436-16 13 

25. Chloroethane GC 601 6200 C2020 

GC/MS 624.1, 6200 8-

0-4127-96 12 

1624B 2020 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7007 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.261</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

26. 2- GC 601 

Chloroethylvinyl ether 

GC/MS 624.1, 

1624B 

27. Chloroform GC 601 6200 C- See footnote 3 p. 

2020 130 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

28. Chloromethane GC 601 6200 C2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

29. 2- GC 612 

Chloronaphthalene 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625B 2020 27 

30. 2-Chlorophenol GC 604 6420 B2021 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

31. 4-Chlorophenyl GC 611 

pheny 1 ether 

GC/MS 625.1, 6410 R- See footnote 8 p. 

16258 2020 27 

32. Chrysene GC 610 
7008 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.262</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

33. GC 610 

Dibenzo( a,h)anthrace 

ne 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

34. GC 601 6200 CDibromochloromethan 2020 

e 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

35. 1,2- GC 601,602 6200 CDichlorobenzene 2020 

GC/MS 624.1, 6200 B- See footnote 8 p. 

1625B 2020 27, 

0-4127-96 12, 0-

4436-16 13 

36. 1,3- GC 601,602 6200 CDichlorobenzene 2020 

GC/MS 624.1, 6200 B- See footnote 8 p. 

1625B 2020 27, 0-4127-96 12 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7009 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.263</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

37. 1,4- GC 601,602 6200 CDichlorobenzene 2020 

GC/MS 624.1, 6200 B- See footnote 8 p. 

1625B 2020 27, 

0-4127-96 12, 0-

4436-16 13 

38. 3,3'- GC/MS 625.1, 6410BDichlorobenzidine 1625B 2020 

IIPLC 605 

39. GC 601 

Dichlorodifluorometh 

ane 

GC/MS 6200 B- 0-4127-96 12, 0-

2020 4436-16 13 

40. 1,1- GC 601 6200 CDichloroethane 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

41. 1,2- GC 601 6200 CDichloroethane 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

42. 1,1- GC 601 6200 CDichloroethene 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 
7010 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.264</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

43. trans-1,2- GC 601 6200 CDichloroethene 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

44. 2,4- GC 604 6420 BDichlorophenol 2021 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625B 2020 27 

45. 1,2- GC 601 6200 CDichloropropane 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12 0-

1624B 2020 4436-16 13 

46. cis-1,3- GC 601 6200 CDich loropropene 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

47. trans-1,3- GC 601 6200 CDichloropropene 2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

48. Diethyl phthalate GC 606 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

49. 2,4- GC 604 6420 BDimethylphenol 2021 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7011 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.265</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625B 2020 27 

50. Dimethyl GC 606 

phthalate 

GC/MS 625.1, 6410 B- See footnote 8 p. 

16258 2020 27 

51. Di-n-butyl GC 606 

phthalate 

GC/MS 625.1, 6410B- See footnote 8 p. 

1625D 2020 27 

52. Di-n-octyl GC 606 

phthalate 

GC/MS 625.1, 6410 Il- See footnote 8 p. 

16258 2020 27 

53. 2, 4-Dinitrophenol GC 604 6420 8- See footnote 8 p. 

2021 27 

GC/MS 625.1, 6410 8-

16258 2020 

54. 2,4-Dinitrotoluene GC 609 

GC/MS 625.1, 6410 8- See footnote 8 p. 

16258 2020 27 

55. 2,6-Dinitrotoluene GC 609 

GC/MS 625.1, 6410 8- See footnote 8 p. 

1625B 2020 27 

56. Epichlorohydrin GC See footnote 3 p. 

130 
7012 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.266</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS See footnote 6 p. 

S102 

57. Ethylbenzene GC 602 6200 C2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

58. Fluoranthene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

59. Fluorene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

60. l,2,3,4,6,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Heptachloro- 14, PAM 16130-

dibenzofuran SSI 15 

61. 1,2,3,4,7,8,9- GC/MS 1613B 9 SGS AXYS 16130 

Heptachloro- 14, PAM 16130-

dibenzofuran SSI 15 

62. 1,2,3,4,6,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Heptach loro-dibenzo- 14, PAM 16130-

p-dioxin SSI 15 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7013 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.267</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

63. GC 612 

Hexachlorobenzene 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

64. GC 612 

Hexachlorobutadiene 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27, 0-4127-96 12 

65. GC 612 

I lexachlorocyclopenta 

diene 

GC/MS 625.1 5, 6410 B- See footnote 8, p. 

1625B 2020 27, 0-4127-96 12 

66. 1,2,3,4,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro- 14, PAM 16130-

dibcnzofuran SSI 15 

67. 1,2,3,6,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro- 14, PAM 16130-

dibenzofuran SSI 15 

68. 1,2,3,7,8,9- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro- 14, PAM 16130-

dibenzofuran SSI 15 

69. 2,3,4,6,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro- 14, PAM 16130-

dibenzofuran SSI 15 
7014 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.268</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

70. 1,2,3,4,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro-dibenzo- 14, PAM 16130-

p-dioxin SSI 15 

71. 1,2,3,6,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro-dibenzo- 14, PAM 16130-

p-dioxin SSI 15 

72. 1,2,3,7,8,9- GC/MS 1613B 9 SGS AXYS 16130 

Hexachloro-dibenzo- 14, PAM 16130-

p-dioxin SSI 15 

73. Hexachloroethane GC 612 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27, 0-4127-96 12 

74. Indeno(l,2,3-c,d) GC 610 

pyrene 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

75. Isophorone GC 609 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

76. Methylene GC 601 6200 C- See footnote 3 p. 

chloride 2020 130 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7015 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.269</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

77. 2-Methyl-4,6- GC 604 6420 Bdinitrophenol 2021 

GC/MS 625.1, 6410B- See footnote 8 p. 

16258 2020 27 

78. Naphthalene GC 610 

GC/MS 625.1, 6410 8- See footnote 8 p. 

16258 2020 27 

HPLC 610 6440 8-

2021 

79. Nitrobenzene GC 609 

GC/MS 625.1, 6410B- Sec footnote 8 p. 

1625B 2020 27 

HPLC D4657-

92 (98) 

80. 2-Nitrophenol GC 604 6420 B2021 

GC/MS 625.1, 6410 8- See footnote 8 p. 

16258 2020 27 

81. 4-Nitrophenol GC 604 6420 B2021 

GC/MS 625.1, 6410B- See foolnote 8 p. 

16258 2020 27 

82. N- GC 607 

Nitrosodimethy lamine 

GC/MS 625.1 5, 6410B- See footnote 8 p. 

1625B 2020 27 
7016 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.270</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

83. N-Nitrosodi-n- GC 607 

propylamine 

GC!MS 625.1 \ 6410 B- See footnote R p. 

16258 2020 27 

84. N- GC 607 

Nitrosodiphenylamine 

GC/MS 625.1 5, 6410 B- See footnote 8 p. 

1625B 2020 27 

85. GC!MS 1613B 9 SGS AXYS 16130 

Octachlorodibenzofur 14, PAM 16130-

an SSI 15 

86. GC!MS 161313 9 SGS AXYS 16130 

Octachlorodibenzo-p- 14, PAM 16130-

dioxin SSI 15 

87. 2,2'-oxybis( I - GC 611 

chloropropane)11 [also 

known as bis(2-

Chloro-1-mcthy lcthy I) 

ether] 

GC!MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

88. 1,2,3,7,8- GC!MS 1613B 9 SGS AXYS 16130 

Pentachloro- 14, PAM 16130-

dibenzofuran SSI 15 

89. 2,3,4,7,8- GC;MS 161313 9 SGS AXYS 16130 

Pentachloro- 14, PAM 16130-

dibenzofuran SSI 15 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7017 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.271</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

90. 1,2,3,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Pentachloro-dibenzo- 14, PAM 16130-

p-dioxin SSI 15 

91. Pentachlorophenol GC 604 6420 B- See footnote 3 p. 

2021 140 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

92. Phenanthrene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

93. Phenol GC 604 6420 B2021 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

94. Pyrene GC 610 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

HPLC 610 6440 B- D4657-

2021 92 (98) 

95. 2,3,7,8- GC/MS 1613B 9 SGS AXYS 16130 

Tetrachloro- 14, PAM 16130-

dibenzofuran SSI 15 
7018 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.272</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

96. 2,3,7,8- GC/MS 613, SGS AXYS 16130 

Tetrachloro-dibenzo- 625.1 5, 14, PAM 16130-

p-dioxin 1613B9 SSI 15 

97. 1,1,2,2- GC 601 6200 C- See footnote 3 p. 

Tetrachloroethane 2020 130 

GC/MS 624.1, 6200 B0-4127-96 12 

1624B 2020 

98. Tetrachloroethene GC 601 6200 C- See footnote 3 p. 

2020 130 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

99. Toluene GC 602 6200 C2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

100. 1,2,4- GC 612 See footnote 3 p. 

Trichlorobenzene 130 

GC/MS 625.1, 6410B- See footnote 8 p. 

16258 2020 27, 0-4127-96 12, 

0-4436-16 13 

101. 1,1,1- GC 601 6200 CTrichloroethane 2020 

GC/MS 624.1, 6200 Il- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

102. 1, 1,2- GC 601 6200 C- See footnote 3 p. 

Trichloroethane 2020 130 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7019 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.273</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

103. Trichloroethene GC 601 6200 C2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

104. GC 601 6200 CTrichlorofluorometha 2020 

ne 

GC/MS 624.1 6200 B- 0-4127-96 12 

2020 

105. 2,4,6- GC 604 6420 BTrichlorophenol 2021 

GC/MS 625.1, 6410 B- See footnote 8 p. 

1625B 2020 27 

106. Vinyl chloride GC 601 6200 C2020 

GC/MS 624.1, 6200 B- 0-4127-96 12, 0-

1624B 2020 4436-16 13 

107. Nonylphenol GC/MS D7065-

17 

108. Bisphenol A GC/MS D7065-

(BPA) 17 

1 09. p-tert- GC/MS D7065-

Octylphenol (OP) 17 
7020 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.274</GPH>

Standard 

Parameter 1 Method EPA 2• 7 Methods 16 ASTM Other 

110. Nonylphenol GC/MS 07065-

M onoethoxylate 17 

(NPlEO) 

111. Nonylphenol GC/MS D7065-

Diethoxylate 17 

(NP2EO) 

112. Adsorbable Adsorptio 1650 10 

Organic Halides n and 

(AOX) Coulometr 

ic 

Titration 

113. Chlorinated In Situ 1653 10 

Phenolics Acetylatio 

n and 

GC/MS 

114. Adsorbable Adsorptio 1621 17 

Organic Fluorine n and 

(AOF) Combustio 

nlon 

Chromatography 

(CIC) 

Table IC notes: 

1 All parameters are expressed in micrograms per liter (μg/L) except for Method 16138, in which the 

parameters are expressed in picograms per liter (pg/L ). 

2 The full Lexl of Methods 601-613, 1613B, 1624B, and 1625B are provided al appendix A, Tesl 

Procedures for Analysis of Organic Pollutants. The standardized test procedure to be used to determine 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7021 


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the method detection limit (MDL) for these test procedures is given at appendix B of this part, Definition 

and Procedure for the Determination of the Method Detection Limit. These methods are available at: 

https://www.epa.gov/cwa-methods as individual PDF files. 

4 Method 624.1 may be used for quantitative determination of acrolein and acry lonitrile, provided that the 

laboratory has documentation to substantiate the ability to detect and quantify these analytes at levels 

necessary to comply with any associated regulations. In addition, the use of sample introduction 

techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 

should be used when analyzing samples for acrolein and acrylonitrile in the absence of such criteria in 

Method 624.1. 

5 Method 625.1 may be extended to include benzidine, hexachlorocyclopentadiene, Nnitrosodimethylamine, N-nitrosodi-n-propylamine, and N-nitrosodiphenylamine. However, when they 

are known to be present, Methods 605, 607, and 612, or Method 16258, are preferred methods for these 

compounds. Method 625.l may be applied to 2,3,7,8-Tetrachloro-dibenzo-p-dioxin for screening 

purposes only. 

6 Selected Analytical Methods Approved and Cited by the United States Environmental Protection 

Agency, Supplement to the 15th Edition of Standard Methods for the Examination of Water and 

Wastewater. 1981. American Public Health Association (APHA). 

7 Each analyst must make an initial, one-time demonstration of their ability to generate acceptable 

precision and accuracy with Methods 601-603, 16248, and 16258 in accordance with procedures 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 624.1 and 625.l 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 quality control (QC) acceptance criteria in the 

pertinent method, analytical results for that parameter in the unspiked sample are suspect. The results 

should be reported but cannot be used to demonstrate regulatory compliance. If the method does not 

contain QC acceptance criteria, control limits of± three standard deviations around the mean of a 

minimum of five replicate measurements must be used. These quality control requirements also apply to 

the Standard Methods, ASTM Methods, and other methods cited. 

8 Method 0-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey 

National Water Quality Laboratory-Determination of Inorganic and Organic Constituents in Water and 

Fluvial Sediments. 1993. USGS. 
7022 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


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9 Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup 

provided the analyst meets the requirements of Method 16l3B (as specified in Section 9 of the method) 

and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and 

Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is 

provided in appendix A to this part and at https://www.epa.gov/cwa-methods/approved-cwa-testmethods-organic-compounds. 

10 Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 

1997 U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS. 

Revision A, 1997 U.S. EPA. The full text for both of these methods is provided at appendix A in part 430 

of this chapter, The Pulp, Paper, and Paperboard Point Source Category. 

11 The compound was fo1merly inaccurately labeled as 2,2'-oxybis(2-chloropropane) and bis(2-

chloroisopropyl) ether. Some versions of Methods 611, and 1625 inaccurately list the analyte as "bis(2-

chloroisopropyl) ether," but use the correct CAS number of 108-60-1. 

12 Method 0-4127-96, U.S. Geological Survey Open-File Report 97-829, Methods of analysis by the 

U.S. Geological Survey National Water Quality Laboratory-Determination of 86 volatile organic 

compounds in water by gas chromatography/mass spectrometry, including detections less than reporting 

limits,1998, USGS. 

13 Method 0-4436-16 U.S. Geological Survey Techniques and Methods, book 5, chap. B 12, 

Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas 

chromatography/mass spectrometry, 2016, USGS. 

14 SGS AXYS Method 16130, "Detetmination of2,3,7,8-Substituted Tetra- through Octa-Chlorinated 

Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using Waters and Agilent Gas ChromatographyTandem-Mass Spectrometry (GC/MS/MS), Revision 1.0" is available at: https://www.sgsaxys.com/wpcontent/uploads/2022/09/SGS-AXYS-Method-16130-Rev-1.0.pdf. 

15 Pace Analytical Method PAM-16130-SSI, "Determination of2,3,7,8-Substituted Tetra- through OctaChlorinated Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using Shimadzu Gas Chromatography 

Mass Spectrometry (GC-MS/MS), Revision 1.1," is available at: pacelabs.com. 

16 Please refer to the following applicable Quality Control Section: Part 6000 Individual Organic 

Compounds, 6020 (2019). The Quality Control Standards are available for download at 

standardmethods.org at no charge. 

17 Method 1621, Determination of Adsorbable Organic Fluorine (AOF) in Aqueous Matrices by 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7023 


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Combustion Ion Chromatography (CIC), January 2024. Available at: https://www.epa.gov/cwa-methods 

Standard 

Parameter Method lliilff;~ Methods 15 ASTM Other 

* * * * * * * 

I

,,,,,,, 

:;o,,,~ Parathion GC 614 6630 B-2021 See footnote 4, page 27; See 

ethyl footnote 3, p. 25. 

GC/MS 625.1 See footnote 11, 0-1126-95. 

* * * * * * * 

Table Id notes: 

1 Pesticides are listed in this table by common name for the convenience of the reader. Additional 

pesticides may be found under Table le of this section, where entries are listed by chemical name. 

2 The standardized test procedure to be used to determine the method detection limit (MDL) for these test 

procedures is given at Appendix B, Defmition and Procedure for the Determination of the Method 

Detection Limit, of this part. 

3 Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and 

Wastewater. September 1978. U.S. EPA. This EPA publication includes thin-layer chromatography (TLC) 

methods. 

4 Methods for the Determination of Organic Substances in Water and Flu vial Sediments, Techniques of 

Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3. 1987. USGS. 

* * * * * 

7 Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable 

precision and accuracy with Methods 608.3 and 625.1 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 608.3 or 5% of all samples analyzed with Method 625.1 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. 

* * * * * 

10 EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods 
7024 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


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for the Determination ofNonconventional Pesticides in Municipal and Industrial Wastewater, EPA 821-R92-002, April 1992, U.S. EPA. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for the 

Determination ofNonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 

821-R-93-0lOB, 1993, U.S. EPA. EPA Method 525.2 is in Determination of Organic Compounds in 

Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass 

Spectrometry, Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods for The 

Determination ofNonconventional Pesticides In Municipal and Industrial Wastewater, Volume I, EPA 

821-R-93-0lOA, 1993, U.S. EPA. Methods 608.3 and 625.1 are available at: cwa-methods/approved-cwatest-methods-organic-compounds. 

11 Method 0-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey 

National Water Quality Laboratory-Determination of pesticides in water by C-18 solid-phase extraction 

and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995. USGS. 

* * * * * 

15 Please refor to the following applicable Quality Control Section: Part 6000 Methods, Individual Organic 

Compounds 6020 (2019). These Quality Control Standards are available for download at 

www.standardmethods.org at no charge. 

* * * * * 

---OF APPROVED TEST PROCEDURES FOR POL YCHLORNA TED BIPHENYL (PCB) 

CONGENERS 

Congener Standard 

Parameter' Number Methodology EPA Methods ASTM Other 

I. 2-\llonochlorobiphenyl PCB-I GC/MS 1628 

2. 3-\llonochlorobiphenyl PCB-2 GC/MS 1628 

3. 4-\llonochlorobiphenyl PCB-3 GC/MS 1628 

4. 2,2'-[)ichlorohiphenyl PCn-4 GC/MS 1628 

5. 2,3-Dichlorobiphenyl PCB-5 GC/MS 1628 

6. 2,3'-Dichlorobiphenyl PCB-6 GC/MS 1628 

7. 2,4-Dichlorobiphenyl PCB-7 GC/MS 1628 

8. 2,4'-Dichlorobiphenyl PCB-8 GC/MS 1628 

9. 2,5-Dichlorohiphenyl PCn-9 GC/MS 1628 

10. 2,6-Dichlorobiphenyl PCB-10 GC/MS 1628 

11. 3 ,3 '-Dichloro bipheny I PCB-11 GC/MS 1628 

12. 3,4-Dichlorobiphenyl PCB-12 GC/MS 1628 

13. 3,4'-Dichlorobiphenyl PCB-13 GC/MS 1628 

14. 3,5-Dichlorobiphcnyl l'CB-14 GC/MS 1628 

15. 4, 4' -Dichloro bipheny I PCB-15 GC/MS 1628 

16. 2,2' ,3-Trichlorobipheny I PCB-16 GC/MS 1628 

17. 2,2' .4-Trichlorobiphenyl PCB-17 GC/MS 1628 

18. 2,2' ,5-Trichlorobiphenyl PCB-18 GC/MS 1628 

19. 2,2' ,6-Trichlorobiphenyl PCB-19 GC/MS 1628 

20. 2,3,3'-Trichlomhiphenyl PCn-20 GC/MS 1628 

21. 2,3,4-Trichlorobiphenyl PCB-21 GC/MS 1628 

22. 2,3,4'-Trichlorobiphenyl PCB-22 GC/MS 1628 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7025 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.279</GPH>

Congener Standard 

Parameter' Nmnber2 Methodology EPA Methods ASTM Other 

23. 2,3 ,5-Trich lorobiphenyl PCB-23 GC/\1S 1628 

24. 2,3 ,6-Trich lorobi phenyl PCB-24 GC/\1S 1628 

25. 2,3 ',4-Trichlorobipheny I PCB-25 GC/\1S 1628 

26. 2,3 ',5-Trichlorobipheny I PCB-26 GC/\1S 1628 

27. 2,3 ',6-Trichlorobiphenyl PCB-27 GC/\1S 1628 

28. 2,4.4'-Trichlorobiphenyl PCB-28 GC/\1S 1628 

29. 2,4,5-Trichlorobiphenyl PCB-29 GC/\1S 1628 

30. 2,4,6-Trichlorobiphenyl PCB-30 GC/\1S 1628 

31. 2,4' ,5-T richlorobipheny I PCB-31 GC/\1S 1628 

32. 2,4',6-'I richlorobiphenyl l'Cl:!-32 UC/\1S 1628 

33. 2' ,3,4-Trichlorobiphenyl PCfl-33 GC/\1S 1628 

34. 2' ,3,5-Trichlorobiphenyl PCB-34 GC/\1S 1628 

35. 3,3 ',4-T richlorobipheny I PCB-35 GC/\1S 1628 

36. 3,3 ',5-T richlorobipheny I PCB-36 GC/\1S 1628 

37. 3,4,4'-Trichlorobiphenyl PCB-37 GC/\1S 1628 

38. 3,4,5-Trich lorobiphenyl PCB-38 GC/\1S 1628 

39. 3,4' ,5-Trichlorobipheny I PCB-39 GC/\1S 1628 

40. 2,2' ,3 ,3 ' -Tetrachloro bi phenyl PCB-40 GC/\1S 1628 

41. 2,2',3 ,4-Tetrachlorobipheny I PCB-41 GC/\1S 1628 

42. 2,2',3,4'-Tetrachlorobiphenyl PCB-42 GC/\1S 1628 

43. 2,2' ,3 ,5-Tctrachlorobiphcnyl PCB-43 GC/\1S 1628 

44. 2,2',:J,5'-Tetrachlorobiphenyl PCfl-44 (JC/\1S 1628 

45. 2,2' ,3 ,6-Tetrachlorobipheny I PCB-45 GC/\1S 1628 

46. 2,2',3,6'-Tetrachlorobiphenyl PCB-46 GC/\1S 1628 

47. 2,2' ,4,4'-Tetrach loro bi phenyl PCB-47 GC/\1S 1628 

48. 2,2' ,4,5-Telrachlorobipheny I PCB-48 GC/\1S 1628 

49. 2,2' ,4,5' -Tetrachloro bi phenyl PCB-49 GC/\1S 1628 

50. 2,2' ,4,6-Tetrachlorobipheny I PCB-50 GC/\1S 1628 

51. 2,2',4,6'-Tetrachlorobiphenyl PCB-51 GC/\1S 1628 

52. 2,2',5,5'-Tetrachlorobiphenyl PCB-52 GC/\1S 1628 

53. 2,2',5,6'-Tetrachlorobiphenyl PCB-53 GC/\1S 1628 

54. 2,2',6,6'-Tetrachlorobiphenyl PCB-54 GC/\1S 1628 

55. 2,3 ,3' ,4-' l' ctrachloro biphcny 1 l'Cl:!-55 GC/\1S 1628 

56. 2,3 ,3' ,4'-Tetrach loro bi phenyl PCfl-56 GC/\1S 1628 

57. 2,3 ,3' ,5-Tetrachl orobiphenyl PCfl-57 GC/\1S 1628 

58. 2,3 ,3' ,5'-Tetrach loro bi phenyl PCB-58 GC/\1S 1628 

59. 2,3 ,3' ,6-Tetrachlorobipheny I PCB-59 GC/\1S 1628 

60. 2,3 ,4,4' -Tetrachloro bipheny I PCB-60 GC/\1S 1628 

61. 2,3 ,4,5-Tetrach lorobiphenyl PCB-61 GC/\1S 1628 

62. 2,3 ,4,6-Tetrach lorobiphenyl PCB-62 GC/\1S 1628 

63. 2,3 .4' ,5-Tetrachlorobiphenyl PCB-63 GC/\1S 1628 

64. 2,3 ,4' ,6-Tetrachlorobipheny I PCB-64 GC/\1S 1628 

65. 2,3 ,5,6-Tetrachlorobiphenyl PCB-65 GC/\1S 1628 

66. 2,3',4,4'-Tctrachlorobiphcnyl PCB-66 GC/\1S 1628 

67. 2,3 ', 4 ,5-' I' etrach I oro bip heny I l'Cl:!-67 UC/\1S 1628 

68. 2,3',4,5'-Tetrachlorobiphenyl PCfl-68 GC/\1S 1628 

69. 2,3 ',4,6-Tetrachlorobipheny I PCB-69 GC/\1S 1628 

70. 2,3 ',4' ,5-Tetrachloro bi phenyl PCB-70 GC/\1S 1628 

71. 2,3 ',4' ,6-Tetrachloro bi phenyl PCB-71 GC/\1S 1628 

72. 2,3',5,5'-Tetrachlorobiphenyl PCB-72 GC/\1S 1628 

73. 2,3 ',5' ,6-Tetrach loro bi phenyl PCB-73 GC/\1S 1628 

74. 2,4.4' ,5-Tetrachlorobiphenyl PCB-74 GC/\1S 1628 

75. 2,4 ,4' ,6-Tetrachlorobiphenyl PCB-75 GC/\1S 1628 

76. 2' ,3,4,5-Tetrachlorobipheny I PCB-76 GCl.\1S 1628 

77. 3,3',4,4'-Tetrachlorobiphenyl PCB-77 GC/.\1S 1628 

78. 3,3',4,5-'J'etrachlorobiphenyl l'Cl:!-78 UC/\1S 1628 

79. 3,3',4,5'-Tetrachlorobiphenyl PCfl-79 GC/\1S 1628 

80. 3,3',5,5'-Tetrachlorobiphenyl PCfl-80 GCl\1S 1628 

81. 3,4,4' ,5-Tetrachlorobipheny I PCB-81 GCl.\1S 1628 

82. 2,2',3 ,3 ',4-Penlachlorobipheny 1 PCB-82 GC/.\1S 1628 

83. 2,2' ,3 ,3 ',5-Pentachlorobipheny I PCB-83 GC/\1S 1628 

84. 2,2' ,3 ,3 ',6-Pentachlorobipheny I PCB-84 GC/\1S 1628 

85. 2,2',3,4,4'-Pentachlorobiphenyl PCB-85 GC/\1S 1628 
7026 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.280</GPH>

Congener Standard 

Parameter' Nmnber2 Methodology EPA Methods ASTM Other 

86. 2,2',3,4,5-Pentachlorobiphenyl PCB-86 GC/\1S 1628 

87. 2,2',3,4,5'-Pentachlorobiphenyl PCB-87 GC/\1S 1628 

88. 2,2',3,4,6-Pentachlorobiphenyl PCB-88 GC/\1S 1628 

89. 2,2' ,3 ,4, 6' -Pentachloro bipheny I PCB-89 GC/\1S 1628 

90. 2,2',3,4',5-Pentachlorobiphenyl PCB-90 GC/\1S 1628 

91. 2,2' ,3, 4' ,6-Pentach I oro bipheny I PCB-91 GC/\1S 1628 

92. 2,2',3,5,5'-Pentachlorobiphenyl PCB-92 GC/\1S 1628 

93. 2,2',3,5,6-Pentachlorobiphenyl PCB-93 GC/\1S 1628 

94. 2,2',3,5,6'-Pentachlorobiphenyl PCB-94 GC/\1S 1628 

95. 2,2' ,3 ,5' ,6-l'entach I oro bipheny I l'Cl:!-95 UC/\1S 1628 

96. 2,2' ,3 ,6,6' -Pen tac h I oro bipheny I PCfl-96 GC/\1S 1628 

97. 2,2',3',4,5-Pentachlorobiphenyl PCB-97 GC/\1S 1628 

98. 2,2',3',4,6-Pentachlorobiphenyl PCB-98 GC/\1S 1628 

99. 2,2',4,4',5-Penlachlorobipheny I PCB-99 GC/\1S 1628 

I 00. 2,2',4,4',6-Pentachlorobiphenyl PCB-100 GC/\1S 1628 

101. 2,2',4,5,5'-Pentachlorobiphenyl PCB-IOI GC/\1S 1628 

102. 2,2',4,5,6'-Pentachlorobiphenyl PCB-102 GC/\1S 1628 

103. 2,2',4,5,'6-Pentachlorobiphenyl PCB-103 GC/\1S 1628 

104. 2,2',4,6,6'-Pentachlorobiphenyl PCB-104 GC/\1S 1628 

I 05. 2,3,3',4,4'-Pentachlorobiphenyl PCB-105 GC/\1S 1628 

106. 2,3,3',4,5-Pcntachlorobiphcnyl PCB-106 GC/\1S 1628 

107. 2,J,J',4',5-Pentachlorohiphenyl PCfl-107 ClC/\1S 1628 

108. 2,3,3',4,5'-Pentachlorobiphenyl PCB-108 GC/\1S 1628 

109. 2,3,3',4,6-Pentachlorobiphenyl PCB-109 GC/\1S 1628 

110. 2,3,3',4',6-Pentachlorobiphenyl PCB-110 GC/\1S 1628 

111. 2,3,3',5,5'-Penlachlorobiphenyl PCB-Ill GC/\1S 1628 

112. 2,3,3',5,6-Pentachlorobiphenyl PCB-112 GC/\1S 1628 

113. 2,3,3',5',6-Pentachlorobiphenyl PCB-113 GC/\1S 1628 

114. 2,3.4,4',5-Pentachlorobiphenyl PCB-114 GC/\1S 1628 

115. 2,3,4,4',6-Pentachlorobiphenyl PCB-115 GC/\1S 1628 

116. 2,3,4,5,6-Pentachlorobiphenyl PCB-116 GC/\1S 1628 

117. 2,3,4',5,6-Pentachlorobiphenyl PCB-117 GC/\1S 1628 

118. 2,3',4,4',5-l'cntachlorobiphcnyl l'CH-118 GC/\1S 1628 

119. 2,3',4,4',6-Pentachlorobiphenyl PCTl-119 GC/\1S 1628 

120. 2,3',4,5,5'-Pentachlorobiphenyl PCTl-120 GC/\1S 1628 

121. 2,3',4,5,'6-Pentachlorobiphenyl PCB-121 GC/\1S 1628 

122. 2' ,3,3',4,5-Penlachlorobipheny I PCB-122 GC/\1S 1628 

123. 2' ,3,4,4',5-Pentachlorobiphenyl PCB-123 GC/\1S 1628 

124. 2' ,3,4,5,5'-Pentachlorobiphenyl PCB-124 GC/\1S 1628 

125. 2',3,4,5,6'-Pentachlorobiphenyl PCB-125 GC/\1S 1628 

126. 3,3 '.4.4' ,5-Pentachlorobipheny I PCB-126 GC/\1S 1628 

127. 3,3',4,5,5'-Pentachlorobiphenyl PCB-127 GC/\1S 1628 

128. 2,2',3,3',4,4'-Hexachlorobiphenyl PCB-128 GC/\1S 1628 

129. 2,2',3,3',4,5-Hcxachlorobiphcnyl PCB-129 GC/\1S 1628 

130. 2,2',3,3',4,5'-l lexachlorobiphenyl l'Cl:!-130 C,C/\1S 1628 

131. 2,2',3,3',4,6-Hexachlorobiphenyl PCTl-131 GC/\1S 1628 

132. 2,2',3,3',4,6'-Hexachlorobiphenyl PCB-132 GC/\1S 1628 

133. 2,2',3,3',5,5'-Hexachlorobiphenyl PCB-133 GC/\1S 1628 

134. 2,2',3,3',5,6-Hexachlorobiphenyl PCB-134 GC/\1S 1628 

135. 2,2',3,3',5,6'-Hexachlorobiphenyl PCB-135 GC/\1S 1628 

136. 2,2',3,3',6,6'-Hexachlorobiphenyl PCB-136 GC/\1S 1628 

137. 2,2',3,4,4' ,5-Hexachlorobiphenyl PCB-137 GC/\1S 1628 

138. 2,2' ,3 ,4 ,4' ,5' -Hexach lorobiphenyl PCB-138 GC/\1S 1628 

139. 2,2',3 ,4.4' ,6-Hexachlorobipheny I PCB-139 GC/.\1S 1628 

140. 2,2' ,3 ,4.4' ,6' -Hexachlorobiphenyl PCB-140 GC/.\1S 1628 

141. 2,2',3,4,5,5'-l lexachlorobiphenyl PCl:!-141 UC/\1S 1628 

142. 2,2',3,4,5,6-Hexachlorobiphenyl PCTl-142 GC/\1S 1628 

143. 2,2',3,4,5,6'-Hexachlorobiphenyl PCTl-143 GCl\1S 1628 

144. 2,2' ,3 ,4,5' ,6-Hexachlorobipheny 1 PCB-144 GC/.\1S 1628 

145. 2,2',3 ,4,6,6'-Hexachlorobipheny 1 PCB-145 GC/.\1S 1628 

146. 2,2',3,4',5,5'-Hexachlorobiphenyl PCB-146 GC/\1S 1628 

147. 2,2',3,4',5,6-Hexachlorobiphenyl PCB-147 GC/\1S 1628 

148. 2,2',3,4',5,6'-Hexachlorobiphenyl PCB-148 GC/\1S 1628 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7027 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.281</GPH>

Congener Standard 

Parameter' Number' Methodology EPA Methods ASTM Other 

149. 2,2',3,4',5',6-Hexachlorobiphenyl PCB-149 GC/MS 1628 

150. 2,2',3,4',6,6'-Hexachlorobiphenyl PCB-150 GC/MS 1628 

151. 2,2',3,5,5',6-Hexachlorobiphenyl PCB-151 GC/MS 1628 

152. 2,2',3,5,6,6'-Hexachlorobiphenyl PCD-152 GC/MS 1628 

153. 2,2',4,4',5,5'-Hexachlorobiphenyl PCB-153 GC/MS 1628 

154. 2,2',4,4',5,6'-Hcxachlorobiphcnyl PCB-154 GC/MS 1628 

155. 2,2',4,4' ,6,6'-Hexachlorobiphenyl PCB-155 GC/MS 1628 

156. 2,3,3',4,4',5-Hexachlorobiphenyl PCB-156 <JC/MS 1628 

157. 2,3,3',4,4',5'-Hexachlorobiphenyl PCB-157 GC/MS 1628 

158. 2,3 ,3' ,4,4' ,6-Hexachlorobipheny 1 PCB-158 GC/MS 1628 

159. 2,3,3',4,5,5'-Hexachlomhiphenyl PCB-159 OC/MS 1628 

160. 2,3,3',4,5,6-Hexachlorobiphenyl PCB-160 GC/MS 1628 

161. 2,3,3',4,5',6-Hexachlorobiphenyl PCD-161 GC/MS 1628 

162. 2,3 ,3' ,4' ,5,5' -Rexach lorobiphenyl PCB-162 GC/MS 1628 

163. 2,3 ,3' ,4' ,5 ,6-Hcxachlorobiphcny 1 PCB-163 GC/MS 1628 

164. 2,3 ,3' ,4' ,5' ,6-Hexachlorobiphenyl PCB-164 GC/MS 1628 

165. 2,3,3',5,5',6-Hexachlorobiphenyl PCB-165 <JC/MS 1628 

166. 2,3,4,4',5,6-Hexachlorobiphenyl PCB-166 GC/MS 1628 

167. 2,3',4,4',5,5'-Hexachlorobiphenyl PCB-167 GC/MS 1628 

168. 2,3',4,4',5',6-Hexachlomhiphenyl PCB-168 OC/MS 1628 

169. 3,3',4,4',5,5'-Hexachlorobiphenyl PCB-169 GC/MS 1628 

170. 2,2',3,3',4,4',5-Heptachlorobiphenyl PCD-170 GC/MS 1628 

171. 2,2'3,3',4,4',6-Heptachlorobiphenyl PCB-171 GC/MS 1628 

172. 2,2',3,3',4,5,5'-Hcptachlorobiphcnyl PCB-172 GC/MS 1628 

173. 2,2',3,3',4,5,6-Heptachlorobiphenyl PCB-173 GC/MS 1628 

174. 2,2',3,3',4,5,6'-Heptachlorobiphenyl PCB-174 GC/MS 1628 

175. 2,2',3,3',4,5',6-Heptachlorubiphenyl PCB-175 GC/MS 1628 

176. 2,2',3,3',4,6,6'-Heptachlorobiphenyl PCB-176 GC/MS 1628 

177. 2,2',3,3',4',5,6-Heptachlomhiphenyl PCB-177 OC/MS 1628 

178. 2,2',3,3',5,5',6-Heptachlorobiphenyl PCB-178 GC/MS 1628 

179. 2,2' ,3,3' ,5 ,6,6' -lleptachlorobipheny I PCD-179 GC/MS 1628 

180. 2,2',3,4,4',5,5'-Heptachlorobiphenyl PCB-180 GC/MS 1628 

181. 2,2',3,4,4',5,6-Hcptachlorobiphcnyl PCB-181 GC/MS 1628 

182. 2,2',3,4,4',5,6'-Heptachlorobiphenyl PCB-182 GC/MS 1628 

183. 2,2',3,4,4',5',6-Heptachlorobiphenyl PCB-183 GC/MS 1628 

184. 2,2',3,4,4',6,6'-Heplachlorobiphenyl PCB-184 GC/MS 1628 

185. 2,2',3,4,5,5',6-Heptachlorobiphenyl PCB-185 GC/MS 1628 

186. 2,2',3,4,5,6,6'-Heptachlombiphenyl PCB-186 GC/MS 1628 

187. 2,2',3,4',5,5',6-Heptachlorobiphenyl PCB-187 GC/MS 1628 

188. 2,2',3,4',5,6,6'-Heptachlorobiphenyl PCB-188 GC/MS 1628 

189. 2,3,3',4,4' ,5,5'-Heptachlorobiphenyl PCB-189 GC/MS 1628 

190. 2,3,3',4,4',5,6-TTeptachlorobiphenyl PCB-190 GC/MS 1628 

191. 2,3,3',4,4',5',6-Heptachlorobiphenyl PCB-191 GC/MS 1628 

192. 2,3,3',4,5,5',6-Heptachlorobiphenyl PCB-192 GC/MS 1628 

193. 2,3,3',4',5,5',6-Heplachlorobiphenyl PCB-193 GC/MS 1628 

194. 2,2',3,3',4,4',5,5'-0ctachlorobiphenyl PCB-194 GC/MS 1628 

195. 2,2',3,3',4,4',5,6-Octachlorohiphenyl PCB-195 GC/MS 1628 

196. 2,2',3,3',4,4',5,6'-0ctachlorobiphenyl PCB-196 GC/MS 1628 

197. 2,2',3,3',4,4',6,6'-0ctachlorobiphenyl PCB-197 GC/MS 1628 

198. 2,2',3,3',4,5,5',6-Octachlorobiphenyl PCB-198 GC/MS 1628 

199. 2,2',3,3',4,5,5',6'-0ctachlorobiphenyl PCD-199 GC/MS 1628 

200. 2,2',3,3',4,5,6,6'-Octachlorobiphenyl PCB-200 GC/MS 1628 

201. 2,2',3,3',4,5',6,6'-0ctachlorobiphenyl PCB-201 GC/MS 1628 

202. 2,2',3,3',5,5',6,6'-0ctachlorobiphenyl PCB-202 GC/MS 1628 

203. 2,2',3,4,4',5,5',6-Octachlorobiphenyl PCB-203 GC/MS 1628 

204. 2,2',3,4,4',5,6,6'-Octachlorobiphenyl PCB-204 GC/MS 1628 

205. 2,3,3',4,4',5,5',6-Octachlorobiphenyl PCB-205 GC/MS 1628 

206. 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl PCB-206 GC/MS 1628 

207. 2,2',3,3',4,4',5,6,6'-Nonachlorobiphenyl PCB-207 GC/MS 1628 

208. 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl PCB-208 GC/MS 1628 

209. Decachlorobiphenyl PCB-209 GC/MS 1628 

210. Total PCBs' Total PCBs GC/MS 1628 
7028 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.282</GPH>

Table Ii notes: 

1 EPA Substance Registry Services name (https://cdxapps.epa.gov/oms-substance-registry-services/) 

2 Preferred abbreviation to facilitate consistency in reporting of the results for these parameters. 

3 Total PCBs is the sum of all the detected congeners in the sample. Calculate the total PCB concentration 

by using zero (0) for the contribution of the congeners that arc not detected. Otherwise, every method blank 

will have a non-zero result, even when no congeners are detected, affecting assessments of the sample 

results relative lo the method blank. Further, there is no method detection limit (MDL) for Total PCBs 

because it is the sum of the results for many individual parameters. Method blanks and samples with no 

detects are reported as "ND" for non-detect for the Total PCBs result ( or a similarly appropriate nonnumeric value). 

-~"'l OF APPROVED TEST PROCEDURES FOR PER-AND POLYFLLORINATED ALKYL 

SUBSTA1'<.:1£S (PFAS) 

Standard 

Pararnetel"1 Abbreviation' Methodology F,PA Methods ASTM3 

1. Perfluorohutanoic acid PrnA LC-MS/MS 1633A 08421-24 

2. Pcrtluoropcntanoic acid PFPcA LC-MS/MS 1633A D8421-24 

3. Pcrfluorohcxanoic acid PFHxA LC-MS/MS 1633A D8421-24 

4. Perfluoroheptanoic acid PFHpA LC-MS/MS 1633A D8421-24 

5. Pertluorooctanoic acid PFOA LC-MS/MS 1633A D8421-24 

6. Perfluorononanoic acid PFNA LC-MS/MS 1633A D8421-24 

7. Perfluorodecanoic acid PFDA LC-MS/MS 1633A D8421-24 

8. Pertluoroundecanoic acid PFUnA LC-MS/MS 1633A D8421-24 

9. Pertluorododecanoic acid PFDoA LC-MS/MS 1633A D8421-24 

10. Perfluorotridecanoic acid PFTrDA LC-MS/MS 1633A D8421-24 

11. Perfluorotetradecanoic acid PFTeDA LC-MS/MS 1633A [)8421-24 

12. Pcrtluorobutancsulfonic acid PFBS LC-MS/MS 1633A D8421-24 

13. Pcrfluoropcntancsulfonic acid PFPcS LC-MS/MS 1633A 08421-24 

14. Pertluorohexanesulfonic acid PFHxS LC-MS/MS 1633A D8421-24 

15. Perfluoroheptanesulfonic acid PFHpS LC-MS/MS 1633A D8421-24 

16. Perfluorooctanesulfonic acid PFOS LC-MS/MS 1633A D8421-24 

17. Perfluorononanesulfonic acid PFNS LC-MS/MS 1633A D8421-24 

18. Perfluorodecanesulfonic acid PFDS LC-MS/MS 1633A D8421-24 

19. Perfluurodudecanesulfonic acid PFDuS LC-MS/MS 1633A D8421-24 

20. 1H,IH,2H,2H-Perfluorohexane sulfonic 4:2FTS LC-MS/MS 1633A D8421-24 

acid 

21. 1H,1H,2H,2H-Perfluorooctane sulfonic 6:2FTS LC-MS/MS 1633A D8421-24 

acid 

22. 1H,1H,2H,2H-Perfluorodecane sulfonic 8:2FTS LC-MS/MS 1633A D8421-24 

acid 

23. Perfluorooctanesulfonamide Pl'OSA LC-MS/MS 1633A D8421-24 

24. N-methyl perfluorooctanesulfonamide NMeFOSA LC-MS/MS 1633A D8421-24 

25. N-ethyl pertluorooctanesulfonamide 'l"EtFOSA LC-MS/MS 1633A D8421-24 

26. N-methyl perfluorooctanesulfonamido- NMeFOSAA LC-MS/MS 1633A D8421-24 

acetic acid 

27. N-ethyl perfluorooctanesulfonamido- NEtFOSJ\.l\. LC-MS/MS 1633A D8421-24 

acetic acid 

28. N-methyl NNfeFOSE LC-MS/MS 1633A D8421-24 

perfluurooctauesulfonamidoethauol 

29. N-ethyl perfluorooctauesulfonamido- NEtFOSE LC-MS/MS 1633A D8421-24 

ethanol 

Other 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7029 

(b) The material listed in this 

paragraph (b) is incorporated by 

reference into this section with the 

approval of the Director of the Federal 

Register under 5 U.S.C. 552(a) and 1 

CFR part 51. All approved incorporation 

by reference (IBR) material is available 

for inspection at the EPA and at the 

National Archives and Records 

Administration (NARA). Contact the 

EPA at: EPA’s Water Docket, EPA West, 

1301 Constitution Avenue NW, Room 

3334, Washington, DC 20004; phone: 

202–566–2426; email: docketcustomerservice@epa.gov. For 

information on the availability of this 

material at NARA, visit 

www.archives.gov/federal-register/cfr/ 

ibr-locations or email fr.inspection@

nara.gov. The material may be obtained 

from the following sources in this 

paragraph (b). 

* * * * * 

(8) * * * 

* * * * * 

BILLING CODE 6560–50–C 

(xi) Method 1621, Determination of 

Adsorbable Organic Fluorine (AOF) in 

Aqueous Matrices by Combustion Ion 

Chromatography (CIC). EPA 821–R–24– 

002. Table Ic. 

(xii) Method 1628 Method 1628 

Polychlorinated Biphenyl (PCB) 

Congeners in Water, Soil, Sediment, 

Biosolids, and Tissue by Low-resolution 

GC/MS using Selected Ion Monitoring. 

July 2021. EPA 821–R–21–002. Table Ii. 

(xiii) Method 1633A Analysis of Perand Polyfluoroalkyl Substances (PFAS) 

in Aqueous, Solid, Biosolids, and Tissue 

Samples by LC–MS/MS. EPA–820–R– 

24–007. Table Ij. 

* * * * * 

(10) American Public Health 

Association, 800 I Street, NW, 

Washington, DC 20001; phone: 202– 

777–2742; website: 

www.standardmethods.org. 

(i) Standard Methods for the 

Examination of Water and Wastewater. 

14th Edition, 1975. Table Ib, Notes 27 

and 86. 

(ii) Standard Methods for the 

Examination of Water and Wastewater. 

15th Edition, 1980, Table Ib, Note 30; 

Table Id. 

(iii) Selected Analytical Methods 

Approved and Cited by the United 

States Environmental Protection 

Agency, Supplement to the 15th Edition 

of Standard Methods for the 

Examination of Water and Wastewater. 

1981. Table Ic, Note 6; Table Id, Note 6. 

(iv) Standard Methods for the 

Examination of Water and Wastewater. 

18th Edition, 1992. Tables Ia, Ib, Ic, Id, 

Ie, and . 

(v) Standard Methods for the 

Examination of Water and Wastewater. 

19th Edition, 1995. Tables Ia, Ib, Ic, Id, 

Ie, and Ih. 

(vi) Standard Methods for the 

Examination of Water and Wastewater. 

20th Edition, 1998. Tables Ia, Ib, Ic, Id, 

Ie, and Ih. 

(vii) Standard Methods for the 

Examination of Water and Wastewater. 

21st Edition, 2005. Table Ib, Notes 17 

and 27. 

(viii) 2120, Color. Revised September 

4, 2021. Table Ib. 

(ix) 2130, Turbidity. Revised 2020. 

Table Ib. 

(x) 2310, Acidity. Revised 2020. Table 

Ib. 

(xi) 2320, Alkalinity. Revised 2021. 

Table Ib. 

(xii) 2340, Hardness. Revised 2021. 

Table Ib. 

(xiii) 2510, Conductivity. Revised 

2021. Table Ib. 

(xiv) 2540, Solids. Revised 2020. 

Table Ib. 

(xv) 2550, Temperature. 2010. Table 

Ib. 

(xvi) 3111, Metals by Flame Atomic 

Absorption Spectrometry. Revised 2019. 

Table Ib. 

(xvii) 3112, Metals by Cold-Vapor 

Atomic Absorption Spectrometry. 

Revised 2020. Table Ib. 

(xviii) 3113, Metals by Electrothermal 

Atomic Absorption Spectrometry. 

Revised 2020. Table Ib. 

(xix) 3114, Arsenic and Selenium by 

Hydride Generation/Atomic Absorption 

Spectrometry. Revised 2020, Table Ib. 

(xx) 3120, Metals by Plasma Emission 

Spectroscopy. Revised 2020. Table Ib. 

(xxi) 3125, Metals by Inductively 

Coupled Plasma-Mass Spectrometry. 

Revised 2020. Table Ib. 

(xxii) 3500-Ca, Calcium. Revised 

2020. Table Ib. 

(xxiii) 3500-Cr, Chromium. Revised 

2020. Table Ib. 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.283</GPH>

Standard 

Parameter' Abbreviation2 Methodology EPA Methods ASTM3 Other 

30. Hexafluoropropylene oxide dimer acid HFPO-DA LC-MS/MS 1633A D8421-24 

31. 4,8-Dioxa-3H-perfluorononanoic acid ADONA LC-MS/MS 1633A D8421-24 

32. Perfluoro-3-methoxypropanoic acid PFMPA LC-MS/MS 1633A D8421-24 

33. Perfluoro-4-methoxybutanoic acid PFMBA LC-MS/MS 1633A D8421-24 

34. Nonafluoro-3,6-dioxaheptanoic acid NFDHA LC-MS/MS 1633A D8421-24 

35. 9-Chlorohexadecafluoro-3-oxanonane-1- 9Cl-PF3ONS LC-MS/MS 1633A D8421-24 

sulfonic acid 

36. 11-Chloroeicosatluoro-3-oxaundecane- 1 ICI-PF3OUdS LC-MS/MS 1633A D8421-24 

1-sulfonic acid 

3 7. Perfluoro(2-ethoxyethane )sulfonic acid PFEESA LC-MS/MS 1633A D8421-24 

38. 3-Perfluoropropyl propanoic acid 3:3FTCA LC-MS/MS 1633A D8421-24 

39. 2H,2H,3H,3H-Pertluorooctanoic acid 5:3FTCA LC-MS/MS 1633A D8421-24 

40. 3-Perfluoroheptyl propanoic acid 7:3FTCA LC-MS/MS 1633A D8421-24 

Table Ij notes: 

1 EPA Substance Registry Services name (https://cdxapps.epa.gov/oms-substance-registry-services/) 

2 Preferred Abbreviation from Method 1633 to facilitate consistency in reporting of the results for these 

parameters. 

3 ASTM D8421-24 is only applicable to aqueous samples. 
7030 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 

(xxiv) 3500–K, Potassium. Revised 

2020. Table Ib. 

(xxv) 3500-Na, Sodium. Revised 2020. 

Table Ib. 

(xxvi) 4110, Determination of Anions 

by Ion Chromatography. Revised 2020. 

Table Ib. 

(xxvii) 4140, Inorganic Anions by 

Capillary Ion Electrophoresis. Revised 

2020. Table Ib. 

(xxviii) 4500 Cl¥, Chloride. Revised 

2021. Table Ib. 

(xxix) 4500-Cl, Chlorine (Residual). 

2011. Table Ib. 

(xxx) 4500–CN¥, Cyanide. Revised 

2021. Table Ib. 

(xxxi) 4500–F¥, Fluoride. Revised 

2021. Table Ib. 

(xxxii) 4500–H+, pH. 2021. Table Ib. 

(xxiii) 4500–H2O2 Hydrogen Peroxide 

(Residual) 2020. Table Ib. 

(xxxiv) 4500–NH3, Nitrogen 

(Ammonia). Revised 2021. Table Ib. 

(xxxv) 4500–NO2

¥, Nitrogen (Nitrite). 

Revised 2021. Table Ib. 

(xxxvi) 4500–NO3

¥, Nitrogen 

(Nitrate). Revised 2019. Table Ib. 

(xxxvii) 4500–N(org), Nitrogen 

(Organic). Revised 2021. Table Ib. 

(xxxviii) 4500–O, Oxygen (Dissolved). 

Revised 2021. Table Ib. 

(xxxix) 4500–P, Phosphorus. Revised 

2021. Table Ib. 

(xl) 4500–PAA Peracetic Acid 

(Residual) 2019. Table Ib. 

(xli) 4500-SiO2, Silica. Revised 2021. 

Table Ib. 

(xlii) 4500–S2¥, Sulfide. Revised 

2021. Table Ib. 

(xliii) 4500–SO3

2¥, Sulfite. Revised 

2021. Table Ib. 

(xliv) 4500–SO4

2¥, Sulfate. Revised 

2021. Table Ib. 

(xlv) 5210, Biochemical Oxygen 

Demand (BOD). Revised 2016. Table Ib. 

(xlvi) 5220, Chemical Oxygen 

Demand (COD). 2011. Table Ib. 

(xlvii) 5310, Total Organic Carbon 

(TOC). Revised 2014. Table Ib. 

(xlviii) 5520, Oil and Grease. Revised 

2021. Table Ib. 

(xlix) 5530, Phenols. Revised 2021. 

Table Ib. 

(l) 5540, Surfactants. Revised 2021. 

Table Ib. 

(li) 6200, Volatile Organic 

Compounds. Revised 2020. Table Ic. 

(lii) 6410, Extractable Base/Neutrals 

and Acids. Revised 2020. Tables Ic and 

Id. 

(liii) 6420, Phenols. Revised 2021. 

Table Ic. 

(liv) 6440, Polynuclear Aromatic 

Hydrocarbons. Revised 2021. Table Ic. 

(lv) 6630, Organochlorine Pesticides. 

Revised 2021. Table Id. 

(lvi) 6640, Acidic Herbicide 

Compounds. Revised 2021. Table Id. 

(lvii) 7110, Gross Alpha and Gross 

Beta Radioactivity (Total, Suspended, 

and Dissolved). 2000. Table Ie. 

(lviii) 7500, Radium. 2001. Table Ie. 

(lix) 9213, Recreational Waters. 2007. 

Table Ih. 

(lxx) 9221, Multiple-Tube 

Fermentation Technique for Members of 

the Coliform Group. Approved 2014. 

Table Ia, Notes 12, 14; and 33; Table Ih, 

Notes 10, 12, and 32. 

(lxi) 9222, Membrane Filter 

Technique for Members of the Coliform 

Group. 2015. Table Ia, Note 31; Table Ih, 

Note 17. 

(lxii) 9223 Enzyme Substrate Coliform 

Test. 2016. Table Ia; Table Ih. 

(lxiii) 9230 Fecal Enterococcus/ 

Streptococcus Groups. 2013. Table Ia, 

Note 32; Table Ih. 

* * * * * 

(15) * * * 

* * * * * 

(lxxi) ASTM D8421–24, Standard Test 

Method for Determination of Per- and 

Polyfluoroalkyl Substances (PFAS) in 

Aqueous Matrices by Co-solvation 

followed by Liquid Chromatography 

Tandem Mass Spectrometry (LC/MS/ 

MS). June 2024. Table Ij. 

* * * * * 

(38) * * * 

(i) Organochlorine Pesticides and 

PCBs in Wastewater Using EmporeTM 

Disk Test Method 3M 0222. Revised 

October 28, 1994. Table Id, Note 8. 

* * * * * 

(e) * * * 

BILLING CODE 6560–50–P 


ddrumheller on DSK120RN23PROD with PROPOSALS1
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7031 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.284</GPH>

TABLE II-REQUIRED CONH.JNERS. PRESERVATION TECHNIQUES. AND HOLDING TIMES 

Maximum 

Parameter number/name Container 1 Preservation l,3 holding time 4 

* * * * * * * 

* * * * * * * 

,,. ";. Ammonia P,FP,G Cool, :s6 °C18, 0.008% 28 days 

Na2S2O3 5, H2SO4 to pH <2 

* * * * * * * 

Table lb Metals7 

* * * * * * * 

FP,G; and FP- 5 mL/L 12NHCL or 5mL/L 90 days. 17 

lined cap17 BrC117 

* * * * * * * * 

II. Phenols G Cool, :s6 °C18, , 0.008% 28 days. 

Na2S2Ol, H2 SO4 to pH <2 

* * * * * * * 

II. Phosphorus, total P, FP,G Cool, ::C:6 °C 18, H2SO4 to 28 days. 

pH <2 2s 

* * * * * * * 

II Hydrogen Peroxide P,G None required Analyze within 15 

minutes. 

Ill Peracetic Acid P,G None required Analyze within 15 

minutes. 

* * * * * * * 

13, 18-20, 22, 24, 25, 27, G, FP-lined 

-~ 

Cool, :s6 °C18, 0.008% 14 days 9 

28, 34-37, 39-43, 45-47, 56, septum Na2S2O35, HCI to pH 29 

76, 97, 98, 101-104, 106. 

Purgeable Halocarbons 

26. 2-Chloroethylvinyl G, FP-lined Cool, :s6 °C18, 0.008% Na2 14 days9 

ether septum S2 035 

6, 57, 99. Purgeable G, FP-lined Cool, :s6 °C18, 0.008% 14 days 9 

aromatic hydrocarbons septum Na2S2O35, HCI to pH 29 

3, 4. Acrolein and G, FP-lined Cool, :s6 °C18, 0.008% 14 days 10 

acry lonitrile septum Na2S2O3, HCl to pH 210 

23,30,44,49,53, 77,80, G, FP-lincd cap Cool, g, °C18, 0.008% 7 days until 

81, 91, 93, 105. Phenols 11 Na2S2O35 extraction, 40 

days after 

extraction 

7, 38. Benzidines 11 12 G, FP-lined cap Cool, ::C:6 °C18, 0.008% Na2 7 days until 

S2 035 extraction. 13 

14, 17, 48, 50-52. Phthalate G, FP-lined cap Cool, ::;6 °C18 7 days until 

esters11 extraction, 40 

days after 

extraction 
7032 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.285</GPH>

Maximum 

Parameter number/name Container 1 Preservation 2,3 holding time 4 

82-84. Nitrosamines1114 G, FP-lined cap Cool, :S6 °C18, store in dark, 7 days until 

0.008% Na2 S2 035 extraction, 40 

days after 

extraction. 

88-94. PCBs11 G, FP-lined cap Cool, Sfi °C18 l year until 

extraction, 1 year 

after extraction. 

54,55, 75, 79 G, FP-lined cap Cool, <6 °C18, store in dark, 7 days until 

Nitroaromatics and 0.008% Na2 S2 Ol extraction, 40 

isophorone11 days after 

extraction. 

I, 2, 5, 8-12, 32, 33, 58, 59, G, FP-lined cap Cool, :S6 °C18, store in dark, 7 days until 

74, 78, 92, 94. Polynuclear 0.008% Na2S2O35 extraction, 40 

aromatic hydrocarbons 11 days after 

extraction 

15, 16, 21, 31, 87. G, FP-lined cap Cool, :S6 °C18, 0.008% Na2 7 days until 

Halocthcrs 11 S2 035 extraction, 40 

days after 

extraction. 

29, 35-37, 63-65, 73, 100. G, FP-lined cap Cool,~ °C18 7 days until 

Chlorinated hydrocarbons 11 extraction, 40 

days after 

extraction 

60-62, 66-72, 85, 86, 88-90, G See footnote 11 See footnote 11 

95, 96. CDDs/CDFs 11 

Aqueous Samples: Field G Cool, :S6 °C18, 0.008% Na2 1 Year. 

and Lab Preservation S2 035, pH <9 

Solids and Mixed-Phase G Cool, :S6 °C18 ?Days. 

Samples: Field 

Preservation 

Tissue Samples: Field G Cool, :S(i °C18 24Hours 

Preservation 

Solids, Mixed-Phase, and G Freeze, ::S-10 °C l Year 

Tissue Samples: Lab 

Preservation 

107-111. Alkylated phenols G Cool, <6 °C, 0.008% 28 days until 

Na2S2O35, H2SO4 to pH <2 extraction, 40 

days after 

extraction 

112. Adsorbable Organic G Cool, <6 °C, 0.008% Hold at least 3 

Halides (AOX) Na2S2O3', HNO3 to pH <2 days, but not more 

than 6 months 

113. Chlorinated Phenolics G, FP-lined cap Cool, <6 °C, 0.008% 30 days until 

Na2S2O35, H2SO4 to pH <2 acetylation, 30 

days after 

acetylation 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7033 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.286</GPH>

Maximum 

Parameter number/name Container 1 Preservation 2•

3 holdine; time 4 

114. Adsorbable Organic HDPE with Cool, <6 °C 90 days 

Fluorine (AOF) linerless HDPE 

or PP caps 26 

* * * * * * * 

Table Ii-Polychlorinated Biphenyl Congener Tests 

1-210. PCB Congeners 

Aqueous Samples: Field G, PP-lined cap Cool, :S6 °C18, 0.008% 1 year 

Preservation Na2S2035 

Solids, Biosolids, and G, PP-lined cap Cool, :S6 °C18 1 year 

Mixed-Phase Samples: 

Field Preservation 

Tissue Samples: Field G, PP-lined cap Cool, :S6 °C18 24 hours 

Preservation 

Solids, Biosolids, G, PP-lined cap Freeze, :5:-10 °C 1 year 

Mixed-Phase, and 

Tissue Samples: Lab 

Preservation 

Sample Extracts G, amber Freeze, < -20 °C 1 year 

Table Ij-Per- and Poly fluorinated Alkyl Substances Tests 

1-40. PFAS 

Aqueous Samples: Field HOPE or PP, Cool, :5:6 °C18 48 hours 

Preservation I inerless cap27 

Solids, Biosolids, and I IDPE, linerless Cool, :S6 °C18 24 hours 28, or 48 

Mixed-Phase Samples: cap27 hours 

Field Preservation 

Tissue Samples: Field HOPE, linerless Cool, :<c:6 °C18, or 24 hours 2~, or 

Preservation cap21 Freeze, :S -20 °C 48 hours 29 

Leachate Samples: Field IIDPE or PP, Cool, :S6 °C18 48 hours 

Preservation I inerless cap27 

Aqueous and Leachate HOPE or PP, Cool, :<c:6 °C18, or 28 days, or 

Samples: Lab I inerless cap27 Freeze, :S -20 °C 90 days 

Preservation 

Solids, Biosolids, and HOPE, linerless Cool, :S6 °C18, or 90 days 

Mixed-Phase Samples: cap21 Freeze, :S -20 °C 

Lab Preservation 

Tissue Samples: Lab HDPE, linerless Freeze, :S -20 °C 90 days 

Preservation cap21 

Sample Extracts Cool, :S6 °C18, or 90 days 

Freeze, :S O °C 

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; 
7034 Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 


ddrumheller on DSK120RN23PROD with PROPOSALS1EP21JA25.287</GPH>

"HDPE" is high density polyethylene; "PP" is polypropylene. 

2 Except where noted in this Table IT 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)(7Xi) 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 "C, 

unless specified othe1wise 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 ofa 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 resu Its equivalent to results produced by arithmetic 

averaging of results of analysis of individual grab samples. For examples of laboratory compositing 

procedures, see EPA Method 1664 Rev. A (oil and grease) and the procedures at 40 CFR 141.24(t)(l4)(iv) 

and (v) (volatile organics). 

3 When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply 

with the Department of Transportation Hazardous Materials Regulations ( 49 CFR pa.rt 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 of0.04% by weight or less (pH 

about 1.96 or greater; Nitric acid (HNO3) in water solutions at concentrations of0.15% by weight or less 

(pH about 1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of0.35% by weight 

or less (pH about 1.15 or greater); and Sodium hydroxide (Na.OH) in water solutions at concentrations of 

0.080% by weight or less (pH about 12.30 or less). 

4 Samples should be analyzed as soon as possible after collection. The times listed are the maximum times 

that samples may be held before the start of analysis and still be considered valid. Samples may be held for 

longer periods only if the permittee or monitoring laboratory have 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 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7035 


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the Regional ATP Coordinator under§ 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 maxinrnm 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 sho1ier 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. 

5 ASTM D7365-09a specifies treatment options for samples containing oxidants (e.g., chlorine) for cyanide 

analyses. Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (23rd 

edition) addresses dechlorination procedures for microbiological analyses. Section A.2 of Standard Method 

4500-NH3 discusses the need for dechlorination of samples for ammonia analysis. Addition of sodium 

thiosulfate to samples for other parameters is only necessary when oxidants are present ( e.g., chlorine). 

* * * * * 

8 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds· 

9 If the sample is not adjusted to pl I 2, then the sample must be analyzed within seven days of 

sampling. 

10 Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling. 

11 When the extractable analytes of concern fall within a single chemical category, the specified 

preservative and maximum holding times should be observed for optimum safeguard of sample 

integrity (i.e., use all necessary preservatives and hold for the shortest time listed). When the 

analytes of concern fall within two or more chemical categories, the sample may be preserved by 
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cooling to S6 °C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and 

adjusting the pH to 6-9; samples preserved in this manner may be held for seven days before 

extraction and for forty days after extraction. Exceptions to this optional preservation and holding 

time procedure are noted in footnote 5 (regarding the requirement for thiosulfate reduction), and 

footnotes 12, 13 (regarding the analysis ofbenzidine). 

12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent 

rearrangement to benzidine. 

13 Extracts may be stored up to 30 days at <0 °C. 

14 For the analysis of diphenylnitrosamine, add 0.008% Na2 S2 03 and adjust pH to 7-10 with NaOH 

within 24 hours of sampling. 

* * * * * 

17 Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 or 

EPA Method 245.7 must be collected in tightly-capped tluoropolymer or glass bottles and preserved with 

BrCl or HCl solution within 48 hours of sample collection. The time to preservation may be extended to 28 

days if a sample is oxidized in the sample bottle. A sample collected for dissolved trace level mercury 

should be filtered in the laboratory within 24 hours of the time of collection. However, if circumstances 

preclude overnight shipment, the sample should be filtered in a designated clean area in the field in 

accordance with procedures given in Method 1669. If sample integrity will not be maintained by shipment 

to and filtration in the laboratory, the sample must be filtered in a designated clean area in the field within 

the time period necessary to maintain sample integrity. A sample that has been collected for determination 

of total or dissolved trace level mercury must be analyzed within 90 days of sample coJlection. 

18 Aqueous samples must be preserved at S 6 °C, and should not be frozen unless data demonstrating that 

sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by 

the regulatory authority. Also, for purposes ofNPDES monitoring, the specification of"S 6 °C" is used in 

place of the "4 °C" and"< 4 °C" sample temperature requirements listed in some methods. It is not 

necessary to measure the sample temperature to three significant figures (11100th of 1 degree); rather, three 

significant figures are specified so that rounding down to 6 °C may not be used to meet the S 6 °C 

requirement. The preservation temperature does not apply to samples that are analyzed immediately (less 

than 15 minutes). 

* * * * * 

25 Samples lo be analyzed for total phosphorous using EPA Method 200. 7 or another approved ICP/ AES 

method may be preserved using nitric acid to pH < 2, or the acid-preserved sample for metals may be used 
Federal Register / Vol. 90, No. 12 / Tuesday, January 21, 2025 / Proposed Rules 7037 

[FR Doc. 2024–29239 Filed 1–17–25; 8:45 am] 

BILLING CODE 6560–50–C 

ENVIRONMENTAL PROTECTION 

AGENCY 

[EPA–HQ–OPP–2024–0562; FRL–12480–01– 

OCSPP] 

40 CFR Part 156 

Pesticides; Petition Seeking 

Rulemaking To Modify Labeling 

Requirements for Pesticides and 

Devices 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Petition for rulemaking. 

SUMMARY: The Environmental Protection 

Agency (EPA) is announcing the 

availability of and seeking public 

comment on a petition received from 

the Attorneys General of the States of 

Nebraska, Iowa, Alabama, Arkansas, 

Georgia, Indiana, 

Louisiana, Montana, North Dakota, 

South Carolina, and South Dakota 

requesting the Agency initiate 

rulemaking to amend the existing 

regulations under the Federal 

Insecticide, Rodenticide, and Fungicide 

Act (FIFRA). The Attorneys General 

believe the Agency should modify its 

requirements such that any state 

labeling requirements inconsistent with 

EPA’s findings and conclusions from its 

human health risk assessment on 

human health effects, such as a 

pesticide’s likelihood to cause cancer, 

birth defects, or reproductive harm, 

constitute misbranding. 

DATES: Comments must be received on 

or before February 20, 2025. 

ADDRESSES: Submit your comments, 

identified by docket identification (ID) 

number EPA–HQ–OPP–2024–0562, by 

one of the following methods: 

• Federal eRulemaking Portal: http:// 

www.regulations.gov. Follow the online 

instructions for submitting comments. 

Do not submit electronically any 

information you consider to be 

Confidential Business Information (CBI) 

or other information whose disclosure is 

restricted by statute. 

• Mail: OPP Docket, Environmental 

Protection Agency Docket Center (EPA/ 

DC), (28221T), 1200 Pennsylvania Ave. 

NW, Washington, DC 20460–0001. 

• Hand Delivery: To make special 

arrangements for hand delivery or 

delivery of boxed information, please 

follow the instructions at http://

www.epa.gov/dockets/contacts.html. 

Additional instructions on 

commenting or visiting the docket, 

along with more information about 

dockets generally, is available at http:// 

www.epa.gov/dockets. 

FOR FURTHER INFORMATION CONTACT: 

Charles Smith, Director, Registration 

Division (7505P), Office of Pesticide 

Programs, Environmental Protection 

Agency, 1200 Pennsylvania Ave. NW, 

Washington, DC 20460–0001; main 

telephone number: (202) 566–1030; 

email address: RDFRNotices@epa.gov. 

SUPPLEMENTARY INFORMATION: 

I. General Information 

A. Does this action apply to me? 

This action is directed to the public 

in general and may be of interest to a 

wide range of stakeholders including 

pesticide registrants, environmental, 

human health, and agricultural 

advocates, pesticide users, and members 

of the public interested in the use of 

pesticides. This listing is not intended 

to be exhaustive but rather provides a 

guide for readers regarding entities 

likely to be affected by his action. 

Because others may also be interested, 

the Agency has not attempted to 

describe all the specific entities that 

may be affected by this action. 

B. What should I consider as I prepare 

my comments for EPA? 

1. Submitting CBI. Do not submit this 

information to EPA through 

Regulations.gov or email. 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 preparing and submitting your 

comments, see the commenting tips at 

https://www.epa.gov/dockets/ 

commenting-epa-dockets. 

II. What action is the Agency taking? 

EPA requests public comment on a 

petition received from several state 

Attorneys General that asks EPA to 

amend 40 CFR 156.10(a)(5) by adding a 

paragraph (xi) to include the following 

as an example of statements or 

representations in the labeling which 

constitute misbranding: ‘‘Statements or 

conclusions regarding the product’s 

human health effects, including the 

likelihood of causing cancer, birth 

defects, or reproductive harm, that are 

different from EPA’s findings and 


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for analysis, and the holding time for total phosphorus may be extended to 6 months. 

26 For AOF, co11ect three separate containers (see Section 8 of Method 1621). 

27 Samples for EPA Method 1633 are collected in HOPE containers with linerless HOPE or PP caps. 

Aqueous samples for ASTM D841-22 are collected in pre-labeled and pre-weighed 15-mL PP tubes. 

Containers for either method must be lot-tested and shown to be free of detectable PF AS. 

28 Samples should be extracted within 24 hours ifNFDHA is a required analyte for a given project. 

29 If the whole fish or other seafood sample is frozen within 48 hours of co11ection, the holding time begins 

when the tissue is processed for analysis ( e.g., fi11eting, grinding, removal of specific tissue for analysis. 

Prepared tissue sample aliquots may be held for up to 90 days when stored at less than or equal to -20 °C.