11200 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Parts 122, 136, 141, 143, 430, 

455, and 465 

[EPA–HQ–OW–2003–0070; FRL–8203–8] 

RIN 2040–AD71 

Guidelines Establishing Test 

Procedures for the Analysis of 

Pollutants Under the Clean Water Act; 

National Primary Drinking Water 

Regulations; and National Secondary 

Drinking Water Regulations; Analysis 

and Sampling Procedures 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Final rule. 

SUMMARY: This rule modifies the testing 

procedures approved for analysis and 

sampling under the Clean Water Act 

and Safe Drinking Water Act. EPA 

proposed these changes for public 

comment on August 18, 2003 and April 

6, 2004. The Clean Water Act changes 

adopted in this final rule fall into the 

following categories: new vendordeveloped methods as well as EPA and 

voluntary consensus standard bodies 

(VCSB) methods, updated versions of 

currently approved methods, revisions 

to method modification and analytical 

requirements, withdrawal of certain 

outdated methods, and changes to 

sample collection, preservation, and 

holding time requirements. This rule 

also changes regulations under the Safe 

Drinking Water Act that establish 

drinking water sampling and analysis 

procedures. The changes include 

approval of vendor-developed methods, 

new EPA and VCSB methods, updated 

VCSB methods, and approval of a 

modification to the test kit used with 

Syngenta Method AG–625 that restricts 

its use in certain circumstances. The 

addition of new and updated methods 

to the wastewater and drinking water 

regulations provides increased 

flexibility to the regulated community 

and laboratories in the selection of 

analytical methods. 

ADDRESSES: EPA has established a 

docket for this action under Docket ID 

No. EPA–OW–2003–0070. All 

documents in the docket are listed on 

the http://www.regulations.gov web site. 

Although listed in the index, some 

information is not publicly available, 

e.g., CBI or other information whose 

disclosure is restricted by statute. 

Certain other material, such as 

copyrighted material, is not placed on 

the Internet and will be publicly 

available only in hard copy form. 

Publicly available docket materials are 

available either electronically through 

http://www.regulations.gov or in hard 

copy at the HQ Water Docket Center, 

EPA/DC, EPA West, Room 3334, 1301 

Constitution Ave., NW., Washington, 

DC. The Public Reading Room is open 

from 8:30 a.m. to 4:30 p.m., Monday 

through Friday, excluding legal 

holidays. The telephone number for the 

Public Reading Room is (202) 566–1744, 

and the telephone number is (202) 566– 

2426 for the HQ Water Docket Center. 

DATES: This regulation is effective April 

11, 2007. The incorporation by reference 

of these methods is approved by the 

Director of the Federal Register on April 

11, 2007. For judicial review purposes, 

this final rule is promulgated as of 1:00 

p.m. (Eastern time) on March 26, 2007 

as provided at 40 CFR 23.2 and 23.7. 

FOR FURTHER INFORMATION CONTACT: For 

information regarding the changes to 

wastewater regulations, contact Meghan 

Hessenauer, Engineering and Analysis 

Division (4303T), USEPA Office of 

Science and Technology, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460, 202–566–1040 (e-mail: 

hessenauer.meghan@epa.gov). For 

information regarding the changes to 

drinking water regulations, contact 

Patricia Snyder Fair, Technical Support 

Center (MS 140), USEPA, Office of 

Ground Water and Drinking Water, 26 

West Martin Luther King Drive, 

Cincinnati, OH 45268, 513–569–7937 (email: fair.pat@epa.gov). 

SUPPLEMENTARY INFORMATION: 

A. Potentially Regulated Entities 

1. Clean Water Act 

EPA Regions, as well as States, 

Territories and Tribes authorized to 

implement the National Pollutant 

Discharge Elimination System (NPDES) 

program, issue permits with conditions 

designed to ensure compliance with the 

technology-based and water qualitybased requirements of the Clean Water 

Act (CWA). These permits may include 

restrictions on the quantity of pollutants 

that may be discharged as well as 

pollutant measurement and reporting 

requirements. If EPA has approved test 

procedures for analysis of a specific 

pollutant, the NPDES permittee must 

use an approved test procedure (or an 

approved alternate test procedure) for 

the specific pollutant when measuring 

the required waste constituent. 

Similarly, if EPA has established 

sampling requirements, measurements 

taken under an NPDES permit must 

comply with these requirements. 

Therefore, entities with NPDES permits 

will potentially be regulated by the 

actions in this rulemaking. Categories 

and entities that may potentially be 

subject to the requirements of today’s 

rule include: 

Category Examples of potentially regulated entities 

State, Territorial, and Indian Tribal 

Governments.

States, Territories, and Tribes authorized to administer the NPDES permitting program; States, Territories, 

and Tribes providing certification under Clean Water Act section 401. 

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

Municipalities ................................... POTWs that must conduct monitoring to comply with NPDES permits. 

This table is not intended to be 

exhaustive, but rather provides a guide 

for readers regarding entities likely to be 

regulated by this action. This table lists 

types of entities that EPA is now aware 

could potentially be regulated by this 

action. Other types of entities not listed 

in the table could also be regulated. To 

determine whether your facility is 

regulated by this action, you should 

carefully examine the applicability 

language at 40 CFR 122.1, (NPDES 

purpose and scope), 40 CFR 136.1 

(NPDES permits and CWA), 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. 

2. Safe Drinking Water Act 

Public water systems are the regulated 

entities required to measure 

contaminants in drinking water 

samples. In addition, EPA Regions, as 

well as States, and Tribal governments 

with authority to administer the 

regulatory program for public water 

systems under the Safe Drinking Water 

Act, may also measure contaminants in 

water samples. When EPA establishes a 

maximum contaminant level (MCL) for 

a given drinking water contaminant, the 

Agency also approves standardized test 

procedures for analysis of the 

contaminant. Public water systems 

required to test water samples must use 


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11201 

one of the approved test procedures. 

Categories and entities that may 

ultimately be subject to the 

requirements of today’s rule include: 

Category Examples of potentially regulated entities NAICS1

State, Local, & Tribal Governments ........... States, local and tribal governments that analyze water samples on behalf of public 

water systems required to conduct such analysis; States, local and tribal governments that themselves operate community and non-transient non-community water 

systems required to monitor.

924110 

Industry ....................................................... Private operators of community and non-transient non-community water systems required to monitor.221310 

Municipalities .............................................. Municipal operators of community and non-transient non-community water systems 

required to monitor.

924110 

1 North American Industry Classification System. 

This table is not intended to be 

exhaustive, but rather provides a guide 

for readers regarding entities likely to be 

regulated by this action. The table lists 

types of entities that EPA is now aware 

could potentially be regulated by this 

action. Other types of entities not listed 

in the table could also be regulated. To 

determine whether your facility is 

regulated by this action, you should 

carefully examine the applicability 

language at 40 CFR 141.2 (definition of 

public water system). If you have 

questions regarding the applicability of 

this action to a particular entity, consult 

the appropriate person listed in the 

preceding FOR FURTHER INFORMATION

CONTACT section. 

B. What Process Governs Judicial 

Review of This Rule? 

Under Section 509(b)(1) of the Clean 

Water Act (CWA), judicial review of 

today’s CWA rule may be obtained by 

filing a petition for review in the United 

States Circuit Court of Appeals within 

120 days from the date of promulgation 

of this rule. For judicial review 

purposes, this final rule is promulgated 

as of 1 p.m. (Eastern time) on March 26, 

2007 as provided at 40 CFR 23.2. Under 

section 1448 (a) of the Safe Drinking 

Water Act (SDWA), judicial review of 

today’s SDWA rule may be obtained by 

filing a petition for review only in the 

United States Court of Appeal for the 

District of Columbia Circuit within 45 

days from the date of promulgation of 

this rule. For SDWA judicial review 

purposes, this final rule is promulgated 

as of 1 p.m. (Eastern time) on March 26, 

2007 as provide at 40 CFR 23.7. The 

requirements of this regulation may also 

not be challenged later in civil or 

criminal proceedings brought by EPA. 

C. Abbreviations and Acronyms Used 

in the Preamble and Final Rule 

AOAC: AOAC-International 

ASTM: ASTM International 

ATP: Alternate Test Procedure 

CWA: Clean Water Act 

EPA: Environmental Protection Agency 

FLAA: Flame Atomic Absorption 

Spectroscopy 

ICP–AES: Inductively Coupled PlasmaAtomic Emission Spectroscopy 

ICP–MS: Inductively Coupled Plasma-Mass 

Spectroscopy 

NPDES: National Pollutant Discharge 

Elimination System 

NPDWR: National Primary Drinking Water 

Regulations 

NSDWR: National Secondary Drinking 

Water Regulations 

QC: Quality Control 

SDWA: Safe Drinking Water Act 

STGFAA: Stabilized Temperature Graphite 

Furnace Atomic Absorption Spectroscopy 

USGS: United States Geological Survey 

VCSB: Voluntary Consensus Standard Body 

D. Table of Contents 

I. Statutory Authority 

A. Clean Water Act 

B. Safe Drinking Water Act 

II. Summary of Final Rule 

A. 40 CFR Part 122 

B. 40 CFR Part 136 

C. 40 CFR Parts 141 and 143 

D. 40 CFR Part 430 

E. 40 CFR Part 455 

F. 40 CFR Part 465 

III. Changes Between the Proposed Rule and 

the Final Rule 

A. Silver Determinations 

B. ASTM Method D5673–02 ‘‘Standard 

Test Method for Elements in Water by 

Inductively Coupled Plasma—Mass 

Spectrometry’’

C. Ammonia Determinations 

D. Available Cyanide Determinations 

E. Kelada-01 Method for Determination of 

Available Cyanide and Total Cyanide 

F. Mandatory Replacement of Mercuric 

Sulfate with Copper Sulfate in Methods 

for Determination of Total Kjeldahl 

Nitrogen 

G. Approval of Additional Standards for 

Turbidity Determinations 

H. Allowed Use of Capillary Columns in 

EPA Methods 601–613, 624, 625, and 

1624B 

I. Changes to Sampling Requirements at 40 

CFR Parts 122, 136, and 403 

J. Approval Status of Total Elements 

Digestion 

K. EPA Method 245.7 for Determination of 

Mercury 

L. Clarification of Reporting Requirements 

M. Corrections to 40 CFR Part 136, Tables 

IA, IB, IC, ID, IE and Footnotes 

N. Revisions to 40 CFR Part 136, Table II 

O. Corrections to Tables 40 CFR 141.23, 

141.24, 141.25, and 141.74 and 

Footnotes 

P. Retention of Syngenta Method AG–625 

for Determination of Atrazine 

Q. EPA Method 327.0 for Determination of 

Chlorine Dioxide 

R. Deferral of Action on Microtox 1010 

IV. Response to Comments 

A. Use of Syngenta Method AG–625 for 

Determination of Atrazine 

B. Results From Use of Revised Methods, 

‘‘The Determination of Radium-226 and 

Radium-228 in Drinking Water by 

Gamma-ray Spectrometry Using HPGE or 

Ge(Li) Detectors.’’ (Revision 1.2, 

December 2004) 

V. Statutory and Executive Order Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review 

B. Paperwork Reduction Act 

C. Regulatory Flexibility Act 

D. Unfunded Mandates Reform Act 

E. Executive Order 13132: Federalism 

F. Executive Order 13175: Consultation 

and Coordination with Indian Tribal 

Governments 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

H. Executive Order 13211: Actions that 

Significantly Affect Energy Supply, 

Distribution, or Use 

I. National Technology Transfer and 

Advancement Act 

J. Congressional Review Act 

I. Statutory Authority 

A. Clean Water Act 

EPA is promulgating today’s rule 

pursuant to the authority of sections 

301(a), 304(h), and 501(a) of the Clean 

Water Act (‘‘CWA’’ or the ‘‘Act’’), 33 

U.S.C. 1311(a), 1314(h), 1361(a). Section 

301(a) of the Act prohibits the discharge 

of any pollutant into navigable waters 

unless the discharge complies with a 

National Pollutant Discharge 

Elimination System (NPDES) permit 

issued under section 402 of the Act. 

Section 304(h) of the Act requires the 

Administrator of the EPA to ‘‘* * * 

promulgate guidelines establishing test 

procedures for the analysis of pollutants 

that shall include the factors which 

must be provided in any certification 


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pursuant to [section 401 of this Act] or 

permit application pursuant to [section 

402 of this Act].’’ Section 501(a) of the 

Act authorizes the Administrator 

to‘‘* * * prescribe such regulations as 

are necessary to carry out this function 

under [the Act].’’ EPA generally has 

codified its test procedure regulations 

(including analysis and sampling 

requirements) for CWA programs at 40 

CFR Part 136, though some 

requirements are codified in other Parts 

(e.g., 40 CFR Chapter I, Subchapters N 

and O). 

B. Safe Drinking Water Act 

The Safe Drinking Water Act (SDWA), 

as amended in 1996, requires EPA to 

promulgate national primary drinking 

water regulations (NPDWRs) that 

specify maximum contaminant levels 

(MCLs) or treatment techniques for 

drinking water contaminants (SDWA 

section 1412 (42 U.S.C. 300g–1)). 

NPDWRs apply to public water systems 

pursuant to SDWA sections 1401(1)(A) 

(42 U.S.C. 300f(1)(A)). According to 

SDWA section 1401(1)(D), NPDWRs 

include ‘‘* * * criteria and procedures 

to assure a supply of drinking water 

which dependably complies with such 

maximum contaminant levels; including 

accepted methods for quality control 

and testing procedures * * *’’ (42 

U.S.C. 300f(1)(D)). In addition, SDWA 

section 1445(a) authorizes the 

Administrator to establish regulations 

for monitoring to help determine 

whether persons are acting in 

compliance with the requirements of the 

SDWA (42 U.S.C. 300j–4). EPA’s 

promulgation of analytical methods for 

NPDWRs is authorized under these 

sections of the SDWA as well as the 

general rulemaking authority in SDWA 

section 1450(a) (42 U.S.C. 300j–9(a)). 

The SDWA also authorizes EPA to 

promulgate national secondary drinking 

water regulations (NSDWRs) for 

contaminants in drinking water that 

primarily affect the aesthetic qualities 

relating to the public acceptance of 

drinking water (SDWA section 1412 (42 

U.S.C. 300g–1)). These regulations are 

not Federally enforceable but are 

guidelines for the States (40 CFR 143.1). 

The NSDWRs also include analytical 

techniques for determining compliance 

with the regulations (40 CFR 143.4). 

EPA’s promulgation of analytical 

methods for NSDWRs is authorized 

under general rulemaking authority in 

SDWA section 1450(a) (42 U.S.C. 300j–

9(a)). 

II. Summary of Final Rule 

The following sections describe the 

changes EPA is making in today’s final 

rule. 

A. 40 CFR Part 122 

1. Some EPA Effluent Guideline 

regulations, as well as EPA’s Sewage 

Sludge Use and Disposal Regulations, 

require the use of analytical methods 

specifically prescribed by the Guideline 

(see e.g. 40 CFR Part 420.21(c)). This 

rule amends the National Pollutant 

Discharge Elimination System (NPDES) 

regulations at 40 CFR Part 122 to clarify 

when an NPDES permittee must use for 

its monitoring and reporting the 

analytical methods specifically required 

in Title 40 of the CFR, Chapter I, 

Subchapters N and O (effluent 

guidelines and sewage sludge, 

respectively) rather than the methods in 

40 CFR Part 136. The regulatory 

language has been amended to explicitly 

require either use of methods at 40 CFR 

Part 136, or other methods that are 

specifically prescribed for the particular 

wastestream or for sewage sludge 

monitoring requirements. 

2. The rule also corrects 

inconsistencies in sampling 

requirements by referencing back to 40 

CFR Part 136 to explicitly require use of 

procedures at 40 CFR Part 136. 

3. Sections 122.21(g)(7), 

122.21(h)(4)(i), and 122.21(j)(4)(viii) 

require an NPDES permit applicant to 

report quantitative data for certain 

pollutants. The rule adds E. coli and 

Enterococci to the list of parameters at 

40 CFR 122.21(g)(7) and 122.21(h)(4)(i), 

and adds E. coli to the list of parameters 

at 40 CFR 122.21(j)(4)(viii). 

B. 40 CFR Part 136 

This rule approves new and revised 

methods for inclusion in 40 CFR Part 

136. Many of those methods are from 

the voluntary consensus standards body 

(VCSB) that publishes Standard 

Methods for the Examination of Water 

and Wastewater. Those ‘‘Standard 

Methods’’ are now available in both 

hard copy and electronic formats. The 

publisher identifies Standard Methods 

in two ways, depending on the medium 

of publication. Hard copy methods are 

identified by the method number (e.g., 

SM 4500–Cl E) and the edition of the 

manual in which they appear (e.g., 18th, 

19th, 20th Editions), while the 

electronic versions available on-line are 

identified by the same method number 

and the year the method was approved 

for release (e.g., 4500–Cl E–00). 

The following discussion briefly 

describes the changes to Part 136 

methods approved today. 

1. This rule amends the regulations at 

40 CFR Part 136 to approve three new 

methods submitted as alternate test 

procedures for monitoring chemical 

pollutants. These methods are ‘‘Test 

Method for Determination of Dissolved 

Inorganic Anions in Aqueous Matrices 

Using Capillary Ion Electrophoresis and 

Chromate Electrolyte’’ (D6508, Rev. 2) 

by Waters Corporation, ‘‘Digestion and 

Distillation of Total Cyanide in Drinking 

and Wastewaters using MICRO DIST 

and Determination of Cyanide by Flow 

Injection Analysis’’ (QuikChem Method 

10–204–00–1–X) by Lachat Instruments, 

and ‘‘Kelada Automated Test Methods 

for Total Cyanide, Acid Dissociable 

Cyanide, and Thiocyanate’’ (Kelada–01) 

by Dr. Nabih Kelada. 

2. The rule approves a broad purpose 

digestion procedure for total recoverable 

elements digestion. EPA is approving 

EPA Method 200.2 (Revision 2.8, 1994) 

for use with Inductively Coupled 

Plasma-Atomic Emission Spectroscopy 

(ICP–AES), Inductively Coupled 

Plasma-Mass Spectroscopy (ICP–MS), 

Stabilized Temperature Graphite 

Furnace Atomic Absorption (STGFAA), 

and Flame Atomic Absorption 

Spectroscopy (FLAA) methods. 

3. The rule approves three new multielement test procedures. The approved 

methods are EPA Method 200.8 

(Revision 5.4, 1994), AOAC Method 

993.14 [16th Edition], and ASTM 

D5673–03 for determination of elements 

by ICP–MS. 

4. EPA is also approving a new multielement test procedure, EPA Method 

200.9 (Revision 2.2, 1994), for 

determination of elements by STGFAA. 

5. The rule approves four new 

methods for determination of 

hexavalent chromium by ion 

chromatography. The methods are EPA 

Method 218.6, AOAC Method 993.23 

[16th Edition], and ASTM D5257–97—

SM 3500–Cr C [20th Edition] and SM 

3500–Cr E [18th, 19th Editions]. 

6. The rule approves five new 

methods for determination of anions by 

ion chromatography. The methods are 

EPA Method 300.0 (Revision 2.1, 1993), 

EPA Method 300.1 (Revision 1.0, 1997), 

AOAC Method 993.30 [16th Edition], 

ASTM D4327, and SM 4110 B [18th, 

19th, and 20th Editions]. 

7. The rule approves the use of six 

automated cadmium reduction methods 

to determine nitrate and nitrite 

individually, as well as in combination. 

The methods are EPA Method 353.2 

(Revision 2.0, 1993), ASTM D3867–99 

(A) and (B), SM 4500–NO3

–E and F 

[18th, 19th, 20th Editions] and 4500–

NO3

–E and F (2000), and USGS Method 

I–4545–85. 

8. The rule approves a new method 

for determination of chlorine by low 

level amperometry—SM 4500–Cl E 

[18th, 19th, 20th Editions] and SM 

4500–Cl E (2000). 


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9. The rule replaces EPA Method 

180.1 (1978) for determination of 

turbidity with EPA Method 180.1 

(Revision 2.0, 1993). 

10. The rule replaces EPA Method 

200.7 (1990) for determination of 

elements by ICP–AES with EPA Method 

200.7 (Revision 4.4, 1994). 

11. The rule replaces EPA Method 

245.1 (1974) for determination of 

mercury with EPA Method 245.1 

(Revision 3.0, 1994). 

12. The rule replaces EPA Method 

335.3 (1978) for determination of total 

cyanide with EPA Method 335.4 

(Revision 1.0, 1993) with a footnote to 

clarify the proper procedure for 

removing sulfide interferences. 

13. The rule replaces EPA Method 

350.1 (1978) for determination of 

ammonia with EPA Method 350.1 

(Revision 2.0, 1993). 

14. The rule replaces EPA Method 

351.2 (1978) for determination of total 

Kjeldahl nitrogen (TKN) with EPA 

Method 351.2 (Revision 2.0 1993). 

15. The rule replaces EPA Method 

353.2 (1978) for determination of 

nitrate-nitrite with EPA Method 353.2 

(Revision 2.0, 1993). 

16. The rule replaces EPA Method 

365.1 (1978) for determination of 

phosphorus (all forms) with EPA 

Method 365.1 (Revision 2.0, 1993). 

17. The rule replaces EPA Method 

375.2 (1978) for determination of sulfate 

with EPA Method 375.2 (Revision 2.0, 

1993). 

18. The rule replaces EPA Method 

410.4 (1978) for determination of 

chemical oxygen demand (COD) with 

EPA Method 410.4 (Revision 2.0, 1993). 

19. The rule replaces EPA Method 

420.2 (1974) for determination of total 

phenols with EPA Method 420.4 

(Revision 1.0, 1993). 

20. The rule approves a new method 

for the determination of mercury, EPA 

Method 245.7 ‘‘Mercury in Water by 

Cold Vapor Atomic Fluorescence 

Spectrometry’’ [Revision 2.0, 2005] 

(EPA–821–R–05–001). 

21. The rule approves a new method 

for determination of available cyanide 

by ligand exchange followed by flow 

injection analysis, ASTM D6888–04. 

22. The rule approves a new method 

for determination of cations by ion 

chromatography, ASTM D6919–03. 

23. The rule approves a new method 

for determination of chloride by 

potentiometry, SM 4500–Cl–D [18th, 

19th, 20th Editions] and SM 4500–Cl–D 

(2000). 

24. The rule approves a new method 

for determination of chloride by ion 

selective electrode, ASTM D512–89 

(1999). 

25. The rule approves two new 

methods for determination of total 

cyanide by ion selective electrode, SM 

4500–CN–F [18th, 19th, 20th Editions] 

and SM 4500–CN–F (2000), and ASTM 

D2036–98 A. 

26. The rule approves two new 

methods for determination of sulfide by 

ion selective electrode, SM 4500–S2

–G 

[18th, 19th, 20th Editions] and ASTM 

D4658–03 (1996). 

27. The rule approves a new method 

for determination of nitrate by ion 

selective electrode, SM 4500–NO3

–[18th, 

19th, 20th Editions] and SM 4500–

NO3

–(2000). 

28. The rule approves an errata sheet 

to correct typographical errors in the 

following methods manuals, ‘‘Shortterm Methods for Estimating the 

Chronic Toxicity of Effluents and 

Receiving Waters to Freshwater 

Organisms,’’ Fourth Edition, U.S. 

Environmental Protection Agency, 

Office of Water, Washington DC, EPA/ 

821/R–02/013 (the ‘‘freshwater chronic 

manual’’), and ‘‘Methods for Measuring 

the Acute Toxicity of Effluents and 

Receiving Waters to Freshwater and 

Marine Organisms,’’ Fifth Edition, U.S. 

Environmental Protection Agency, 

Office of Water, Washington DC, EPA/ 

821/R–02/012 (the ‘‘freshwater acute 

manual’’). 

29. The rule approves the use of 

newer versions of 74 methods published 

by ASTM International. The new 

versions are published in the 1994, 

1996, and 1999 Annual Book of ASTM 

Standards Vols. 11.01 and 11.02, in the 

2000 Annual Book of ASTM Standards, 

Vol. 11.02 and in individual standards 

published after 2000. 

30. The rule approves the use of 

newer versions of 88 methods published 

by the Standard Methods Committee 

and adopts a new numbering system to 

track the approved versions of Standard 

Methods. The new versions are 

published in Standard Methods Online 

(APHA 2003). 

31. The rule approves the use of 

newer versions of 19 methods published 

by AOAC–International. The new 

versions of these methods are published 

in Official Methods of Analysis of 

AOAC–International, 16th Edition, 

1995. 

32. The rule approves the replacement 

of the mercuric sulfate catalyst with 

copper sulfate in methods approved for 

the determination of total Kjeldahl 

nitrogen (TKN). 

33. The rule approves the use of 

styrene divinyl benzene beads and 

stabilized formazin as alternatives to the 

presently approved formazin standard 

for determination of turbidity. 

34. As described in the preamble to 

the April 2004 proposed rule (69 FR 

18213), EPA is adopting a new § 136.6 

to introduce greater flexibility in the use 

of approved methods. The section 

describes the circumstances in which 

approved methods may be modified and 

the requirements that analysts must 

meet to use these modified methods in 

required measurements without prior 

EPA approval. The rule also includes 

language at § 136.6(c) to clarify that 

analysts need only meet method 

performance requirements for target 

analytes (those analytes being measured 

for NPDES reporting) when using multianalyte methods for compliance 

monitoring purposes. The rule also 

includes the language at § 136.6(d) to 

allow explicitly the use of capillary 

(open tubular) GC columns with EPA 

Methods 601–613, 624, 625, and 1624B 

as alternatives to the packed GC 

columns specified in those methods, 

provided that analysts generate new 

retention time tables with capillary 

columns to be kept on file with other 

information for review by auditors. 

35. The rule withdraws 109 methods 

contained in EPA’s ‘‘Methods for the 

Chemical Analysis of Water and 

Wastes’’ for which approved 

alternatives published by voluntary 

consensus standards bodies (e.g., ASTM 

and Standard Methods) are available. 

36. The rule withdraws liquid-liquid 

extraction (LLE) methods, including 

EPA Methods 612 and 625, as approved 

procedures for determination of 1,2- 

dichlorobenzene, 1,3-dichlorobenzene, 

and 1,4-dichlorobenzene. 

37. The rule withdraws approval of all 

oil and grease methods that use 

chlorofluorocarbon-113 (CFC–113; 

Freon–113) as an extraction solvent. 

38. The rule revises Table II (Required 

Containers, Preservation Techniques, 

and Holding Times) and the footnotes to 

the table at 40 CFR 136.3(e). The table 

and footnotes specify approved 

sampling, preservation, and holding 

time requirements for the methods 

approved for compliance monitoring to 

reduce confusion, resolve any conflicts 

with instructions in the underlying 

compliance monitoring method, and 

reflect current understanding of sample 

preservation requirements. The most 

significant of the changes are those 

made to Footnote 6, which addresses 

the preservation of samples to be 

analyzed for cyanide. Based on 

information gathered during the 

development of new cyanide methods 

approved in this rulemaking, and 

information collated from various 

commenters and experts in cyanide 

analyses, EPA revised footnote 6 to 

Table II by adding text that describes 

procedures that are recommended for 

removal or suppression of cyanide 

interferences, including interferences 


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from sulfur, sulfide, sulfite, thiocyanate, 

and aldehydes. The recommended 

procedures may differ from those 

described in the older approved 

methods. 

39. EPA is changing ‘‘Director of the 

Environmental Monitoring Systems 

Laboratory’’ and ‘‘Director, Analytical 

Methods Staff’’ to ‘‘Alternate Test 

Procedure Program Coordinator, 

Washington, DC’’ every place the 

phrases appear in the regulations. This 

reflects the current organizational 

structure and title for the head of EPA’s 

Alternate Test Procedure (ATP) Program 

management. In addition, addresses for 

submission of ATPs are being updated 

to reflect the current location of the 

Alternate Test Procedure Program 

Coordinator. 

40. The rule makes other minor 

editorial revisions to clarify existing 

regulations. 

C. 40 CFR Parts 141 and 143 

1. This rule amends the regulations at 

40 CFR Part 141 and Part 143 to allow 

the use of 66 methods in ’’Standard 

Methods Online’’ (APHA 2003) (40 CFR 

141.21, 141.23, 141.74, and 143.4). 

2. This rule allows the use of 28 

newer versions of methods published by 

ASTM International. The new versions 

are published in the 1999 ‘‘Annual Book 

of ASTM Standards,’’’ Vols.11.01 and 

11.02, in the 2000 ‘‘Annual Book of 

ASTM Standards,’’ Vol. 11.02 and in 

individual standards published after 

2000 (40 CFR 141.23). 

3. This rule approves a new method 

submitted as an alternate test procedure 

for the determination of common 

anions—chloride, fluoride, nitrate, 

nitrite, orthophosphate, and sulfate, 

‘‘Test Method for Determination of 

Dissolved Inorganic Anions in Aqueous 

Matrices Using Capillary Ion 

Electrophoresis and Chromate 

Electrolyte’’ (D6508, Rev. 2) by Waters 

Corporation (40 CFR 141.23 and 143.4). 

4. This rule approves two new 

methods for determination of available 

cyanide, ‘‘Available Cyanide by Flow 

Injection, Ligand Exchange, and 

Amperometry,’’ Method OIA–1677, DW 

(January 2004), and ASTM D6888–04 

(40 CFR 141.23). 

5. This rule approves the use of EPA 

Method 300.1 (Revision 1.0, 1997) for 

compliance determinations of chloride, 

fluoride, nitrate, nitrite, orthophosphate, 

and sulfate (40 CFR 141.23 and § 143.4). 

6. This rule approves the use of EPA 

Method 552.3 (Revision 1.0, 2003) for 

compliance determinations of dalapon 

(40 CFR 141.24). 

7. This rule amends 40 CFR 141.25 to 

add a new method for determination of 

radium-226 and radium-228. This 

method, ‘‘The Determination of Radium226 and Radium-228 in Drinking Water 

by Gamma-ray Spectrometry Using 

HPGE or Ge(Li) Detectors’’ (Revision 

1.2, December 2004), was developed by 

the Environmental Resources Center at 

the Georgia Institute of Technology, and 

was originally submitted to EPA as an 

alternate test procedure to the currently 

approved methods for determination of 

radium-226 and radium-228. 

8. This rule allows States the option 

of approving ITS Free chlorine test 

strips as a test kit for the measurement 

of free chlorine using ‘‘Free Chlorine 

Species’’ (HOCl- and OCl-) by Test 

Strip,’’ ITS Method D99–003 (Revision 

3.0, November 21, 2003) by Industrial 

Test Systems, Inc. (40 CFR 141.74). 

9. This rule approves EPA Method 

327.0 (Revision 1.1, 2005) for 

measurement of chlorine dioxide 

residuals (40 CFR 141.74). 

10. This rule approves the use of 

styrene divinyl benzene beads and 

stabilized formazin as alternatives to the 

presently approved formazin standard 

for determination of turbidity (40 CFR 

141.74). 

11. This rule revises footnote 17 to the 

table at 40 CFR 141.23 to allow the use 

of a 450–W UV lamp in the Kelada 

Method-01 for determination of cyanide. 

12. This rule allows the use of 

Syngenta Method AG–625, with the 

modified immunoassay testing product 

manufactured by Beacon Analytical 

Systems, for the measurement of 

atrazine under certain conditions. It 

may only be used by those systems that 

do not use chlorine dioxide for drinking 

water treatment. In addition, the results 

of the analysis of samples with 

concentrations of atrazine more than 

one-half the atrazine MCL (i.e., more 

than 1.5 μg/L) must be confirmed using 

another approved method (40 CFR 

141.24). 

13. This rules also revises footnote 8 

to the table in paragraph (a)(1) to correct 

a long-standing discrepancy between 

the footnote and the specifications in 

Standard Method 9221 E. The table in 

question lists Standard Method 9221 E 

as one of two procedures that may be 

used for monitoring fecal coliforms. 

Footnote 8 simply notes the holding 

time for the A–1 broth used in this 

procedure. Today’s action corrects the 

holding time specified in the footnote 8 

to match the 7-day holding time that is 

specified in Standard Method 9221 E 

(40 CFR 141.74) 

D. 40 CFR Part 430 

This rule amends the Effluent 

Limitations Guidelines for the pulp, 

paper, and paperboard point source 

category at 40 CFR Part 430 to approve 

a new method for determination of 

chlorinated phenolics in wastewaters 

generated by these industries. The rule 

adds a new section, 430.02(g), to allow 

the use of ‘‘Chlorinated Phenolics in 

Water by In situ Acetylation and GC/MS 

Determination’’ (Method CP–86.07) 

developed by the National Council for 

Air and Stream Improvement (NCASI) 

as an alternative to otherwise required 

Method 1653 in Part 430, Appendix A. 

E. 40 CFR Part 455 

This rule amends the regulations at 40 

CFR Part 455 by moving Table 7 from 

40 CFR Part 455 to 40 CFR Part 136.3(a) 

as new Table IG. 

F. 40 CFR Part 465 

This rule amends the Effluent 

Limitations Guidelines for the coil 

coating point source category at 40 CFR 

Part 465 to replace the method listed at 

section 465.03(c) for determination of 

oil and grease in wastewater samples 

from all subcategories of coil coating 

with EPA Method 1664A for 

determination of non-polar materials 

(NPM), which is generally equivalent to 

total petroleum hydrocarbons. 

III. Changes Between the Proposed Rule 

and the Final Rule 

Except as noted below, the content of 

the final rule is the same as that of the 

proposed rule. In some instances, EPA 

revised for clarity the language of the 

final rule from that in the proposed rule. 

A. Silver Determinations 

EPA received comments on the 

Agency’s proposed withdrawal of EPA 

Method 272.1 which included 

information on how to keep silver in 

solution in samples with known or 

suspected high levels of silver by adding 

a solution containing cyanogen 

chloride. As a result, EPA has added a 

footnote to Table IB at § 136.3 to include 

procedures for preparation and addition 

of this reagent to digested samples of 

this type to keep the silver in solution 

for analysis by any of the approved 

methods. The Agency is withdrawing 

EPA Method 272.1, as proposed in April 

2004 (69 FR 18183 April 6, 2004). 

B. ASTM Method D5673–02 ‘‘Standard 

Test Method for Elements in Water by 

Inductively Coupled Plasma—Mass 

Spectrometry’’ 

Based on comment received on the 

Agency’s proposed approval of ASTM 

Method D5673–02, EPA is approving an 

updated version of this method ASTM 

D5673–03. EPA included the updated 

version of this method in a notice of 

data availability (70 FR 7909, February 

16, 2005) and requested public 


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comment on whether it should be 

approved. EPA received no adverse 

comments. 

C. Ammonia Determinations 

EPA received comment on the 

Agency’s proposed approval of an 

updated version of EPA Method 350.1. 

The commenter stated that mandating 

the use of ethylene-diamine-tetra-acetate 

(EDTA) in the method could adversely 

affect method performance when using 

an automated analyzer and submitted 

data to support this claim. Based on 

EPA’s review of the data, the Agency is 

adding a footnote to Table IB at § 136.3 

allowing analysts to omit EDTA from 

EPA Method 350.1, provided that all of 

the quality control (QC) acceptance 

criteria in the method are met. 

D. Available Cyanide Determinations 

The Agency solicited comment 

regarding problems encountered with 

the use of ligand exchangeamperometric detection methods for 

determination of available cyanide in 

samples that contain significant 

amounts of solids and solicited 

potential solutions to these problems. 

Based on public comment, EPA is 

adding a footnote to Table IB at § 136.3 

that includes suggestions for sample 

filtration and for limiting the time 

between addition of ligand exchange 

reagents and analysis to solve these 

problems when necessary. The Agency 

proposed ASTM Method D6888–03 for 

determining available cyanide. Since 

publication of the proposal, EPA has 

received a revised version of this 

method. EPA included this revised 

version in a Notice of Data Availability 

(NODA) and requested public comment 

on the approval of this revised version 

of the method (70 FR 7909, February 16, 

2005). D6888–04 contains a new online 

sulfide removal procedure and 

represents a refinement to the proposed 

version. EPA received no adverse 

comments on this revised version of the 

method and is approving ASTM Method 

D6888–04 in today’s rule. 

E. Kelada-01 Method for Determination 

of Available Cyanide and Total Cyanide 

Based on a comment and data 

received on the Agency’s proposed 

approval of the Kelada-01 method for 

determination of available cyanide and 

total cyanide for use in NPDES 

compliance monitoring, a note has been 

added at 40 CFR 136.3, Table IB, 

Footnote 55 to allow the use of 450–W 

UV lamp instead of the 550–W lamp 

specified in the method if it provides 

performance within the quality control 

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. The Agency also is adding the 

note at 40 CFR 141.23, Footnote 17, as 

this method was previously approved 

for use in drinking water compliance 

monitoring. 

F. Mandatory Replacement of Mercuric 

Sulfate With Copper Sulfate in Methods 

for Determination of Total Kjeldahl 

Nitrogen 

The Agency proposed the mandatory 

replacement of mercury sulfate with 

copper sulfate in total Kjeldahl nitrogen 

(TKN) digestion. Comments expressed 

concern that copper sulfate will provide 

inferior performance in some samples, 

and suggested that EPA allow the 

continued use of mercury sulfate in 

analyses, offering copper sulfate as an 

option. Based on EPA’s evaluation of 

these comments, the Agency has 

decided that it will continue to allow 

the use of mercury sulfate in TKN 

analyses. 

G. Approval of Additional Standards for 

Turbidity Determinations 

Based on comments received on the 

proposed approval of additional 

standards for use in methods to 

determine turbidity, the Agency is 

replacing turbidity standard trade 

names with more generic listings in the 

footnote to Table IB at § 136.3. An 

example formulation for each generic 

listing is also included in order to 

provide a reference to at least one 

source of the generic standard material. 

The Agency also is adding a similar 

footnote to the table in 40 CFR 141.74 

where the approved methods for the 

determination of turbidity in drinking 

water are listed. 

H. Allowed Use of Capillary Columns in 

EPA Methods 601–613, 624, 625, and 

1624B 

The Agency proposed new language 

that explicitly allows the use of 

capillary columns in place of packed 

columns with EPA Methods 601–613, 

624, 625, and 1624B, provided that all 

QC tests in these methods are performed 

and all QC acceptance criteria are met. 

Based on comments received on this 

proposal, EPA is clarifying the 

regulations at § 136.6 to state that 

retention times will change with the 

switch from packed to capillary 

columns, so analysts are not required to 

meet the retention times specified in the 

method when the switch is made. 

Instead, analysts must generate new 

retention time tables with capillary 

columns to be kept on file with other 

information for review by auditors. 

I. Changes to Sampling Requirements at 

40 CFR Parts 122, 136, and 403 

The Agency proposed changes to the 

sampling requirements specified at 40 

CFR Parts 122, 136 and 403. Based on 

comments received on these proposed 

updates, the sampling requirements 

have been modified to include clarifying 

language with respect to grab and 

composite sampling requirements, and 

to add E. coli and Enterococci to the 

parameters listed at Part 122.21 for 

which an NPDES applicant must 

provide analytical information. In 

addition, on October 14, 2005, EPA 

published in the Federal Register final 

changes to its General Pretreatment 

Regulations (70 FR 60134). In these 

regulations, EPA consolidated 

monitoring requirements for indirect 

dischargers into 40 CFR 403.12(g). In the 

proposal for the current rule, EPA 

proposed to modify 40 CFR 403.12 (b). 

Based on changes made to 40 CFR Part 

403 on October 14, 2005, however, the 

proposed modifications to CFR 403.12 

(b) are no longer required. 

J. Approval Status of Total Elements 

Digestion 

The Agency proposed to approve a 

‘‘total recoverable’’ elements digestion 

procedure, and also to retain ‘‘total’’

elements digestion for graphite furnace 

atomic absorption (GFAA) analyses. 

Based on comments received on this 

proposal, EPA is clarifying the language 

in Table IB at § 136.3 to specify Section 

4.1.3 of Methods for Chemical Analysis 

of Water and Wastes (MCAWW) as the 

approved digestion procedure for use 

with non-platform graphite furnace 

atomic absorption determinations. 

K. EPA Method 245.7 for Determination 

of Mercury 

The Agency proposed approval of 

EPA Method 245.7 (December 2003) as 

an additional method for determination 

of mercury. Based on comments 

received on this proposal, EPA has 

revised the method and is approving 

EPA Method 245.7 (Revision 2.0, 2005) 

in this rule. Specifically, EPA has 

approved the method with the following 

changes: includes a discussion of the 

gas-liquid separator in Section 2.6, 

reduces the amount of hydrochloric acid 

used during sample digestion, includes 

the addition of hydrochloric acid (HCl) 

to standard solutions, clarifies that 

additional procedures for handling 

difficult matrices may be used provided 

that laboratories meet the method 

performance criteria, and revises 

procedures for preparing reagent blanks 

to remove the addition of stannous 

chloride (SnCl2) and include addition of 


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HCl. EPA also has corrected section 

numbering and references throughout 

Sections 4 and 7 of the method. 

L. Clarification of Reporting 

Requirements 

The Agency proposed to add a new 

§ 136.7 that would clarify that a quality 

control (QC) failure does not relieve a 

permittee of the duty to report results 

and that results are to be reported to the 

level specified in the method or 

required in the permit, whichever is 

lower. EPA agrees with public comment 

that the proposed revision was unclear. 

In this rule, EPA is revising this action 

to clarify our intent in text at § 136.3, 

rather than take final action on the 

proposed text at § 136.7. 

EPA proposed a new § 136.7 

amendment to resolve conflicts between 

current reporting requirements at 40 

CFR Parts 122 and 125 and preservation 

requirements at 40 CFR 136.3(e) and 

instructions in compliance monitoring 

methods specified in the tables at 40 

CFR 136.3(a). For example, some 

methods provide ‘‘reject tests’’ (e.g. 

Method 5210 B 5-day BOD, section 6a, 

Standard Methods, 20th edition) or state 

that a ‘‘result may not be reported for 

regulatory compliance purposes’’ (e.g. 

Method OIA 1677: Available Cyanide, 

section 9.3.4, OI Analytical) if an 

analytical quality control measure is 

outside its control limit range 

(acceptance criteria). However, it may 

be necessary to report such results if 

resampling, reanalysis or other 

corrective action is not possible. Not 

reporting these results may cause a 

permittee to be in violation of Part 122 

or 125 reporting requirements. 

Reporting such available data is 

recommended as a good laboratory 

practice (D3856–95 Standard Guide for 

Good Laboratory Practices in 

Laboratories Engaged in Sampling and 

Analysis of Water, Annual Book of 

ASTM Standards, Water and 

Environmental Technology, Vol 11.01 

Water (I), p. 353, 2003). 

For clarification, in this rule, EPA is 

adding a statement to the text preceding 

Tables IA to IG at § 136.3(a), and Table 

II at § 136.3(e) to state that reporting 

requirements of Parts 122 or 125 may 

take precedence over the otherwise 

applicable reporting or preservation 

requirements of a particular analytical 

method. 

M. Corrections to 40 CFR Part 136, 

Tables IA, IB, IC, ID, IE and Footnotes 

The Agency is correcting errors that 

were published in the proposed Table 

IA (List of Approved Biological 

Methods), Table IB (List of Approved 

Inorganic Test Procedures), Table IC 

(List of Approved Test Procedures for 

Non-Pesticide Organic Compounds), 

Table ID (List of Approved Test 

Procedures for Pesticides), and Table IE 

(List of Approved Radiologic Test 

Procedures) and the footnotes to those 

tables. 

N. Revisions to 40 CFR Part 136, Table 

II 

The rule revises Table II (Required 

Containers, Preservation Techniques, 

and Holding Times), and the footnotes 

to Table II at 40 CFR 136.3(e). The 

action of updating Table II at § 136.3(e) 

reflects EPA’s evaluation of comments 

received on the April 6, 2004 proposal. 

EPA revised footnote 1 to more clearly 

distinguish between polyethylene (P), 

fluoropolymer (FP), glass (G), and lowdensity polyethylene (LDPE) and has 

made it explicit that a sample to be used 

to determine fluoride is to be collected 

in a polyethylene bottle. EPA revised 

footnotes 2 and 7 to add language to 

make more clear that preservation must 

be within 15 minutes after collection of 

a grab sample, a composite sample, or 

an aliquot split from a composite 

sample collected automatically over 

time. 

EPA modified footnote 4 to clarify the 

start of holding times for the different 

types of sample collection (grab 

samples, composite samples collected 

automatically, and a set of grab samples 

that is composited in the laboratory). 

The revisions remove the requirement 

for collection of samples to determine 

cyanide in amber glass bottles with 

PTFE-lined caps from footnote 6. 

Footnotes 5 and 6 describe procedures 

recommended for removal or 

suppression of cyanide interferences, 

including interferences from oxidants, 

sulfide, sulfite, thiocyanate, and 

aldehydes. In addition, the footnote also 

provides that other procedures for 

removal or suppression of cyanide 

interferences may be employed, 

provided the analyst demonstrates that 

such other procedures more accurately 

measure cyanide. 

EPA clarified requirements in 

footnote 17 specific to sampling for 

trace mercury, added EPA Method 245.7 

to footnote 17, and removed footnote 17 

from the ‘‘Preservation’’ and ‘‘Maximum 

Holding Time’’ headers. EPA has 

clarified footnote 18 to indicate that the 

number of significant figures is intended 

to establish an absolute upper limit on 

sample temperature and preclude 

meeting the specification through 

rounding of numbers and added an 

exception to footnote 18 for a sample 

analyzed immediately (in less than 15 

minutes from collection). EPA deleted 

footnote 19 because the information is 

now in footnote 5. Deletion of this 

footnote resulted in renumbering all of 

the subsequent footnotes to Table II. 

EPA has also clarified that 

preservation is not required for soil and 

sediment samples. EPA also has revised 

preservation requirements for acrolein, 

acrylonitrile, and purgeable aromatics to 

remove inconsistences, revised 

requirements for collection of samples 

to be tested for Cryptosporidium and 

Giardia, and established 0–8 °C as the 

holding temperature for samples to be 

tested for Cryptosporidium. In addition, 

the Agency is correcting minor 

formatting and typographical errors that 

were published in the proposed Table II. 

EPA recognizes that the requirements 

at § 136.3 may differ from those 

described in some older approved 

methods and today’s action clarifies that 

this section supersedes instructions in a 

compliance method. Where there are 

conflicts with existing methods 

published by EPA, VCSBs, or other 

entities, we expect that the next 

revisions of these methods will conform 

to the requirements at § 136.3(e). 

O. Corrections to Tables 40 CFR Parts 

141.23, 141.24, 141.25, and 141.74 and 

Footnotes 

The final rule corrects a number of 

errors in the proposed tables at § 141.23 

(Inorganic Chemical Sampling and 

Analytical Requirements), 141.24 

(Organic Chemicals, Sampling and 

Analytical Requirements), 141.25 

(Analytical Methods for Radioactivity) 

and 141.74 (Analytical and Monitoring 

Requirements) and the footnotes to 

those tables. The Agency also revised 

the wording of several entries for the 

cyanide methods in the tables at 40 CFR 

141.23 to more clearly distinguish 

among the various methodologies listed 

in those tables. 

P. Retention of Syngenta Method AG–

625 for Determination of Atrazine 

The Agency proposed to withdraw 

approval of Syngenta Method AG–625 

for the determination of atrazine in 

drinking water. Based on comments 

received regarding the April 6, 2004 

proposal and comments received 

regarding additional data submitted in 

response to the Notice of Data 

Availability (70 FR 7909, February 16, 

2005), EPA has decided to retain 

Syngenta Method AG–625 with some 

restrictions on its use. The revised 

approval requires confirmation of any 

compliance monitoring results for 

atrazine that are greater than one half of 

the MCL for atrazine, using an alternate 

approved method. EPA based its 

approval on the use of the modified 

immunoassay testing product produced 


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by Beacon Analytical Systems, the only 

version of the product that is currently 

offered for sale. However, use is not 

authorized for public water systems 

which use chlorine dioxide for drinking 

water treatment. 

Q. EPA Method 327.0 for Determination 

of Chlorine Dioxide 

The Agency proposed to approve EPA 

Method 327.0 (Revision 1.0, 2003) for 

the determination of chlorine dioxide 

(40 CFR 141.74). In the final rule, the 

Agency has approved EPA Method 

327.0 (Revision 1.1, 2005) and corrected 

three typographical errors in the 

proposed method. 

R. Deferral of Action on Microtox 1010 

Because EPA is continuing to evaluate 

public comment about use of the 

Microtox 1010 test procedure for 

determinations of acute whole effluent 

toxicity, and the data supporting use of 

this test procedure, EPA is not taking 

final action on the proposal to approve 

Microtox 1010 for compliance 

monitoring. 

IV. Response to Comments 

EPA received two comments 

regarding methods included in this final 

rule from the August 18, 2003 proposal 

(68 FR 49548), 115 comments on the 

April 6, 2004 proposal (69 FR 18166), 

and nine comments on the February 16, 

2005 Notice of Data Availability 

(NODA) (70 FR 7909). Commenters 

represented a number of different 

interests, including analytical 

laboratories, water utilities, instrument 

manufacturers, State and local 

governments, trade associations, 

scientists, and private citizens. A 

summary of major public comments on 

the proposed rules and the NODA and 

the Agency’s responses is presented in 

this section, and section III of this 

preamble. The public docket for this 

rule includes the Agency’s response to 

all comments. 

A. Use of Syngenta Method AG–625 for 

Determination of Atrazine 

EPA proposed withdrawing approval 

of Syngenta Method AG–625 (Syngenta 

Crop Protection Inc.) for the 

determination of atrazine. Based on 

comments and additional data 

submitted in response to the NODA, 

EPA has decided to retain Syngenta 

Method AG–625 as an approved method 

for atrazine, subject to certain 

conditions. Today’s amended rule will 

require the use of an alternate approved 

method for atrazine to confirm any 

results from the Syngenta method that 

are greater than one half of the MCL for 

atrazine. EPA’s decision to retain the 

approval of Method AG–625 is based on 

using the modified immunoassay testing 

product manufactured by Beacon 

Analytical Systems (Atrazine Plate Kit–

Cat# CPP–004), the only version of the 

product currently offered for sale. 

However, based on data submitted in 

response to the NODA, EPA is not 

approving Method AG–625 for use 

when chlorine dioxide is used for 

drinking water treatment. 

One commenter supported the 

withdrawal of Syngenta Method AG–

625, citing EPA’s Environmental 

Technology Verification (ETV) study, 

and suggested that the method had not 

been validated adequately prior to 

EPA’s earlier approval. The commenter 

also suggested that approval of a 

modified version of AG–625 may be 

preferable, but was concerned that the 

method using the original testing 

product could lead to reports of noncompliance and/or increased treatment 

cost based on erroneous atrazine 

measurements in the interim. 

Other comments questioned the 

validity of data submitted by the 

American Water Works Association 

(AWWA) that demonstrated method 

deficiencies and requested that the data 

not be considered by EPA. The 

commenters noted that data were not 

accompanied by suitable quality control 

checks and that some tests (i.e., testing 

the effect of humic acid) were not 

reproducible in later studies by the 

same investigator. The commenters also 

suggested that data generated by AWWA 

was not generated according to Method 

AG–625, but rather by simply using the 

commercial testing product without 

reference to the method. 

As reported by Adams (Adams et al., 

JAWWA, 2004, pp. 126–139), the 

original immunoassay test kit used with 

Method AG–625 was subject to a 

positive bias in the measurement of 

atrazine in the presence of disinfectants 

used in drinking water treatment, such 

as chlorine, monochloroamine, 

chloramine T, chlorine dioxide and 

other substances. Additionally, data 

reported by Adams using the modified 

Beacon test kit, data from the 

Environmental Technology Verification 

(ETV) Program, and, in fact, data in the 

December 2004 Syngenta study 

(Atrazine: Final Report, Syngenta 

Number T006141–04, 12/10/2004), 

demonstrate that test kits marketed by 

Beacon, Abraxis, and SDI show a 

modest positive bias in raw and finished 

drinking water for most samples (i.e., 

the measured concentrations in most 

samples were higher than the expected 

values). For a distinct minority of 

samples in these two studies, no bias or 

a negative bias was shown (i.e., the 

measured concentrations were equal to 

or lower than the expected 

concentrations in a few samples). The 

December 2004 Syngenta study 

submitted to EPA demonstrated that the 

modified Beacon immunoassay test kit 

performed suitably in the presence of 

chlorine, monochloroamine, chloramine 

T, chloroform, and humic acid. 

However the data show that an 

interference occurred in the presence of 

chlorine dioxide unless samples were 

analyzed within one day of collection. 

EPA agrees that data from both 

Syngenta and AWWA (Adams) indicate 

that, except for cases involving chlorine 

dioxide, the modified testing product 

performed substantially better with 

regard to the positive bias and 

interferences than did the original 

product in the presence of disinfectants 

and other interferences. EPA also agrees 

that, in general, the immunoassay 

products examined in these studies 

exhibit some positive bias for atrazine. 

Low results were only obtained from 

analyses of a few samples. 

EPA recognizes that a potential 

positive bias is a concern for water 

utilities, particularly those located in 

areas such as the Midwest, where 

atrazine is used extensively to control 

weeds in corn and sorghum crops. 

However, in many other areas, where it 

is not used, atrazine is not likely to be 

found in drinking water samples at all. 

Because accurate information on the 

occurrence of contaminants at 

concentrations close to the MCL is 

necessary for EPA to meet its obligation 

to review MCLs every six years, EPA has 

retained approval of Syngenta Method 

AG–625 for atrazine with the conditions 

on its use described below. The 

following conditions have been added 

as Footnote 5 to the table at 40 CFR 

141.24(e)(1). 

‘‘This method may not be used for the 

analysis of atrazine in any system where 

chlorine dioxide is used for drinking water 

treatment. In samples from all other systems, 

any result for atrazine generated by Method 

AG–625 that is greater than one-half the 

maximum contaminant level (MCL) (i.e., 

greater than 0.0015 mg/L or 1.5 μg/L) must 

be confirmed using another approved method 

for this contaminant and should use 

additional volume of the original sample 

collected for compliance monitoring. In 

instances where a result from Method AG–

625 triggers such confirmatory testing, the 

confirmatory result is to be used to determine 

compliance.’’

The MCL for atrazine is 0.003 mg/L 

(3 μg/L). Thus, any results from Method 

AG–625 greater than 0.0015 mg/L (1.5 

μg/L) must be confirmed through the 

use of another approved method for 

atrazine. In such instances, the 


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confirmatory result is used to determine 

compliance, because the methods used 

for confirmatory testing are considered 

more accurate. 

EPA acknowledges that this 

requirement for confirmation may cause 

some utilities to choose not to employ 

Method AG–625. However, the approval 

of a method at 40 CFR Part 141 does not 

constitute a requirement for its use 

when other approved methods are 

available. Furthermore, EPA has 

concluded that, given the distribution of 

atrazine use nationwide, the majority of 

water utilities will not be negatively 

affected by the confirmation 

requirement and can take advantage of 

the potential cost savings afforded by 

Method AG–625 relative to other 

approved methods for atrazine. EPA 

notes that if utilities are monitoring for 

a broad range of contaminants using 

approved methods that cover multiple 

analytes (e.g., Method 525.2), then the 

use of a test kit may not offer a cost 

advantage because of the ability to 

include atrazine in a broad spectrum 

method. 

Based on the data provided in 

response to the proposed rule and 

NODA, EPA agrees that the presence of 

chlorine dioxide has substantial 

potential to interfere with Method AG–

625. Therefore, EPA has not approved 

the method for use in water systems 

where chlorine dioxide is used for 

drinking water treatment. While the 

data from one study suggest that the 

atrazine results are not affected if 

samples are analyzed within 24 hours 

after sample collection, the 

circumstances surrounding this 

observation in the study have not been 

fully characterized. At a future date, 

EPA may reconsider the use of Method 

AG–625 by water systems using 

chlorine dioxide, if more information is 

available characterizing the performance 

of the method. 

B. Results From Use of Revised 

Methods, ‘‘The Determination of 

Radium-226 and Radium-228 in 

Drinking Water by Gamma-ray 

Spectrometry Using HPGE or Ge(Li) 

Detectors.’’ (Revision 1.2, December 

2004) 

The final rule establishing 

radionuclide drinking water standards 

published on December 7, 2000 (65 FR 

76708) required drinking water systems 

to sample and report on radionuclides 

in their drinking water supplies during 

the period from December 8, 2003 to 

December 31, 2007, including the 

combined result for radium-226 and 

radium-228. Prior to today’s rule, 

separate methods were required for the 

measurement of radium-226 and 

radium-228. The separate results of the 

two isotopes are summed to provide the 

‘‘combined’’ result that is compared to 

the MCL. One commenter supported the 

approval of the method from the Georgia 

Institute of Technology because one 

method can be used to measure both 

radium isotopes and would make for a 

faster result. The commenter also noted 

that there are approximately 150,000 

Public Water Supply source water taps 

across the country that would have to be 

sampled. Given these monitoring 

requirements, the commenter was 

concerned about sufficient laboratory 

capacity to meet the monitoring 

requirements of the December 2000 rule 

because approval of the Georgia 

Institute of Technology method would 

not become effective until promulgation 

of today’s rule. 

In response to this comment, EPA is 

allowing community water systems to 

use samples collected after January 1, 

2005 and analyzed using the analytical 

method approved in this rule to satisfy 

the radium-226 and radium-228 

monitoring requirements for the 2005–

2007 compliance period. (Minor 

corrections to the method were made in 

December 2004 and are reflected in the 

version approved in this rule, so it was 

not available for analyzing samples 

collected prior to 2005.) Allowing this 

early use of the method should alleviate 

some of the laboratory capacity 

concerns. EPA has included a footnote 

in the revised table of analytical 

methods for radioactivity at § 141.25 to 

indicate that samples analyzed using the 

newly approved method are acceptable. 

Such ‘‘grandfathered’’ data must be 

based on results from the analytical 

method approved for use by this final 

rule. The term ‘‘grandfathered data’’

used in this rule does not apply to data 

collected to meet other grandfathering 

provisions specified in the radionuclide 

final rule that was published on 

December 7, 2000 (65 FR 76708). 

V. Statutory and Executive Order 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review 

Under Executive Order 12866 (58 FR 

51735, October 4, 1993), the Agency 

must determine whether the regulatory 

action is ‘‘significant’’ and therefore 

subject to OMB review and the 

requirements of the Executive Order. 

The Executive Order defines 

‘‘significant regulatory action’’ as one 

that is likely to result in a rule that may: 

(1) Have an annual effect on the 

economy of $100 million or more, or 

adversely affect in a material way the 

economy, a sector of the economy, 

productivity, competition, jobs, the 

environment, public health or safety, or 

State, local, or Tribal governments or 

communities; 

(2) Create a serious inconsistency or 

otherwise interfere with an action taken 

or planned by another agency; 

(3) Materially alter the budgetary 

impact of entitlements, grants, user fees, 

or loan programs or the rights and 

obligations of recipients thereof; or 

(4) Raise novel legal or policy issues 

arising out of legal mandates, the 

President’s priorities, or the principles 

set forth in the Executive Order. 

It has been determined that this rule 

is not a ‘‘significant regulatory action’’

under the terms of Executive Order 

12866 and is therefore not subject to 

OMB review. 

B. Paperwork Reduction Act 

This action does not impose an 

information collection burden under the 

provisions of the Paperwork Reduction 

Act, 44 U.S.C. 3501 et seq. This rule 

does not impose any information 

collection, reporting, or recordkeeping 

requirements. This rule merely adds 

new and updated versions of testing 

procedures, withdraws some older 

testing procedures, and establishes new 

sample collection, preservation, and 

holding time requirements. 

Burden means the total time, effort, or 

financial resources expended by persons 

to generate, maintain, retain, or disclose 

or provide information to or for a 

Federal agency. This includes the time 

needed to review instructions; develop, 

acquire, install, and utilize technology 

and systems for the purpose of 

collecting, validating, and verifying 

information, processing and 

maintaining information, and disclosing 

and providing information; adjust the 

existing ways to comply with any 

previously applicable instructions and 

requirements; train personnel to be able 

to respond to a collection of 

information; search data sources; 

complete and review the collection of 

information; and transmit or otherwise 

disclose the information. 

An Agency may not conduct or 

sponsor, and a person is not required to 

respond to a collection of information 

unless it displays a currently valid OMB 

control number. The OMB control 

numbers for EPA’s regulations in 40 

CFR are listed in 40 CFR Part 9. 

C. Regulatory Flexibility Act 

The RFA generally requires an agency 

to prepare a regulatory flexibility 

analysis of any rule subject to notice 

and comment rulemaking requirements 

under the Administrative Procedure Act 

or any other statute unless the agency 


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11209 

certifies that the rule will not have a 

significant economic impact on a 

substantial number of small entities. 

Small entities include small businesses, 

small organizations, and small 

governmental jurisdictions. 

For purposes of assessing the impacts 

of this rule on small entities for methods 

under the Clean Water Act, small entity 

is defined as: (1) A small business as 

defined by the Small Business 

Administration’s (SBA) regulations at 13 

CFR 121.201; (2) a small governmental 

jurisdiction that is a government of a 

city, county, town, school district or 

special district with a population less 

than 50,000; and (3) a small 

organization that is any not-for-profit 

enterprise which is independently 

owned and operated and is not 

dominant in its field. The RFA provides 

default definitions for each type of small 

entity. It also authorizes an agency to 

use alternative definitions for each 

category of small entity, ‘‘which are 

appropriate to the activities of the 

agency’’ after proposing the alternative 

definition(s) in the Federal Register and 

taking comment (5 U.S.C. 601(3)–(5)). In 

addition to the above, to establish an 

alternative small business definition, 

agencies must consult with SBA’s Chief 

Counsel for Advocacy. 

For purposes of assessing the impacts 

of this rule on small entities for methods 

under the Safe Drinking Water Act, EPA 

considered small entities to be public 

water systems serving 10,000 or fewer 

persons. This is the cut-off level 

specified by Congress in the 1996 

Amendments to the Safe Drinking Water 

Act for small system flexibility 

provisions. In accordance with the RFA 

requirements, EPA proposed using this 

alternative definition in the Federal 

Register (63 FR 7620, February 13, 

1998), requested public comment, 

consulted with the Small Business 

Administration, and expressed its 

intention to use the alternative 

definition for all future drinking water 

regulations in the Consumer Confidence 

Reports regulation (63 FR 44511, August 

19, 1998). As stated in that final rule, 

the alternative definition would be 

applied to this regulation as well. 

After considering the economic 

impacts of today’s final rule on small 

entities, I certify that this action will not 

have a significant economic impact on 

a substantial number of small entities. 

This action approves new and updated 

versions of testing procedures, 

withdraws some older testing 

procedures, and approves new sample 

collection, preservation, and holding 

time requirements. Generally, these 

changes will have a positive impact on 

small entities by increasing method 

flexibility, thereby allowing entities to 

reduce costs by choosing more costeffective methods. In some cases, 

analytical costs may increase slightly 

due to the additional QC requirements 

included in the methods that are being 

approved to replace older EPA methods. 

However, most laboratories that analyze 

samples for EPA compliance monitoring 

have already instituted QC requirements 

as part of their laboratory practices. We 

have determined that a small number of 

small entities that are still using the 

CFC–113 based oil and grease methods 

may need to devote resources to analyst 

training when they switch to hexanebased methods. However, due to the 

decreased availability of CFC–113 in the 

marketplace, we anticipate that the cost 

differential, if any, will soon favor the 

use of the hexane-based methods. The 

phaseout of CFC–113 based methods is 

required to comply with the Montreal 

Protocol which prohibits the use of 

CFC–113 based methods after December 

31, 2005. 

Although this final rule will not have 

a significant economic impact on a 

substantial number of small entities, 

EPA nonetheless has tried to reduce the 

impact of this rule on small entities. 

Anticipating the prohibition of CFC–113 

based methods, EPA promulgated 

hexane-based methods in May 1999. 

EPA has determined that most 

laboratories have now switched to 

hexane-based oil and grease methods, 

making the analysis costs competitive 

with the CFC–113 based methods. 

D. Unfunded Mandates Reform Act 

Title II of the Unfunded Mandates 

Reform Act of 1995 (UMRA), Public 

Law 104–4, establishes requirements for 

Federal agencies to assess the effects of 

their regulatory actions on State, Tribal, 

and local governments and the private 

sector. Under section 202 of the UMRA, 

EPA generally must prepare a written 

statement, including a cost-benefit 

analysis, for proposed and final rules 

with ‘‘Federal mandates’’ that may 

result in expenditures to State, local, 

and Tribal governments, in the 

aggregate, or to the private sector, of 

$100 million or more in any one year. 

Before promulgating an EPA rule for 

which a written statement is needed, 

section 205 of the UMRA generally 

requires EPA to identify and consider a 

reasonable number of regulatory 

alternatives and adopt the least costly, 

most cost-effective or least burdensome 

alternative that achieves the objectives 

of the rule. The provisions of section 

205 do not apply when they are 

inconsistent with applicable law. 

Moreover, section 205 allows EPA to 

adopt an alternative other than the least 

costly, most cost-effective or least 

burdensome alternative if the 

Administrator publishes with the final 

rule an explanation of why that 

alternative was not adopted. 

Before EPA establishes any regulatory 

requirements that may significantly or 

uniquely affect small governments, 

including Tribal governments, it must 

have developed under section 203 of the 

UMRA a small government agency plan. 

The plan must provide for the 

notification of potentially affected small 

governments, enabling officials of 

affected small governments to have 

meaningful and timely input in the 

development of EPA regulatory 

proposals with significant Federal 

intergovernmental mandates, and 

informing, educating, and advising 

small governments on compliance with 

the regulatory requirements. 

This rule contains no Federal 

mandates (under the regulatory 

provisions of Title II of UMRA) for 

State, local, or Tribal governments or 

the private sector. The rule imposes no 

enforceable duty on any State, local, or 

Tribal governments or the private sector. 

In fact, this rule should (on the whole) 

save money for governments and the 

private sector by increasing method 

flexibility, and allowing these entities to 

reduce monitoring costs by taking 

advantage of innovations. Thus, today’s 

rule is not subject to the requirements 

of Sections 202 and 205 of the UMRA. 

EPA has determined that this rule 

contains no regulatory requirements that 

might significantly or uniquely affect 

small governments. Generally, this 

action will have a positive impact by 

increasing method flexibility, thereby 

allowing method users to reduce costs 

by choosing more cost effective 

methods. In some cases, analytical costs 

may increase slightly due to changes in 

methods, but these increases are neither 

significant nor unique to small 

governments. This rule merely approves 

new and updated versions of testing 

procedures, withdraws some older 

testing procedures, and approves new 

sample collection, preservation, and 

holding time requirements. Thus, 

today’s rule is not subject to the 

requirements of Section 203 of UMRA. 

E. Executive Order 13132: Federalism 

Executive Order 13132, entitled 

‘‘Federalism’’ (64 FR 43255, August 10, 

1999), requires EPA to develop an 

accountable process to ensure 

‘‘meaningful and timely input by State 

and local officials in the development of 

regulatory policies that have federalism 

implications.’’ ‘‘Policies that have 

federalism implications’’ is defined in 

the Executive Order to include 


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11210 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

regulations that 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.’’

This final rule does not have 

federalism implications. It will not have 

substantial direct effects on the States, 

on the relationship between the national 

government and the States, or on the 

distribution of power and 

responsibilities among the various 

levels of government, as specified in 

Executive Order 13132. This rule merely 

approves new and updated versions of 

testing procedures, withdraws some 

older testing procedures, and approves 

new sample collection, preservation, 

and holding time requirements. The 

costs to State and local governments 

will be minimal (in fact, governments 

may see a cost savings), and the rule 

does not preempt State law. Thus, 

Executive Order 13132 does not apply 

to this rule. 

In the spirit of Executive Order 13132, 

and consistent with EPA policy to 

promote communications between EPA 

and State and local governments, EPA 

specifically solicited comment on the 

proposed rule from State and local 

officials. 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

Executive Order 13175, entitled 

‘‘Consultation and Coordination with 

Indian Tribal Governments’’ (65 FR 

67249, November 9, 2000), requires EPA 

to develop an accountable process to 

ensure ‘‘meaningful and timely input by 

tribal officials in the development of 

regulatory policies that have tribal 

implications.’’

This final rule does not have tribal 

implications, as specified in Executive 

Order 13175. It will not have substantial 

direct effects on Tribal governments, on 

the relationship between the Federal 

government and Indian tribes, or on the 

distribution of power and 

responsibilities between the Federal 

government and Indian tribes. This rule 

merely approves new and updated 

versions of testing procedures, 

withdraws some older testing 

procedures, and approves new sample 

collection, preservation, and holding 

time requirements. The costs to Tribal 

governments will be minimal (in fact, 

governments may see a cost savings), 

and the rule does not preempt State law. 

Thus, Executive Order 13175 does not 

apply to this rule. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

Executive Order 13045: ‘‘Protection of 

Children from Environmental Health 

Risks and Safety Risks’’ (62 FR 19885, 

April 23, 1997) applies to any rule that: 

(1) Is determined to be ‘‘economically 

significant’’ as defined under Executive 

Order 12866, and (2) concerns an 

environmental health or safety risk that 

EPA has reason to believe may have a 

disproportionate effect on children. If 

the regulatory action meets both criteria, 

the Agency must evaluate the 

environmental health or safety effects of 

the planned rule on children, and 

explain why the planned regulation is 

preferable to other potentially effective 

and reasonably feasible alternatives 

considered by the Agency. This final 

rule is not subject to the Executive 

Order 13045 because it is not 

economically significant as defined in 

Executive Order 12866. Further it does 

not concern an environmental health or 

safety risk that EPA has reason to 

believe may have a disproportionate 

effect on children. This action approves 

new and updated versions of testing 

procedures, withdraws some older 

testing procedures, and approves new 

sample collection, preservation, and 

holding time requirements. 

H. Executive Order 13211: Actions That 

Significantly Affect Energy Supply, 

Distribution, or Use 

This rule is not subject to Executive 

Order 13211, ‘‘Actions Concerning 

Regulations That Significantly Affect 

Energy Supply, Distribution, or Use’’ (66 

FR 28355 (May 22, 2001)) because it is 

not a significant regulatory action under 

Executive Order 12866. 

I. National Technology Transfer and 

Advancement Act 

Section 12(d) of the National 

Technology Transfer and Advancement 

Act of 1995, (NTTAA), Public Law 104–

113, section 12(d) (15 U.S.C. 272 note), 

directs EPA to use voluntary consensus 

standards in its regulatory activities 

unless to do so would be inconsistent 

with applicable law or otherwise 

impractical. Voluntary consensus 

standards are technical standards (e.g., 

material specifications, test methods, 

sampling procedures, and business 

practices) that are developed or adopted 

by voluntary consensus standard bodies. 

The NTTAA directs EPA to provide 

Congress, through the OMB, 

explanations when the Agency decides 

not to use available and applicable 

voluntary consensus standards. This 

final rule approves the use of over 150 

standards developed by Standard 

Methods and ASTM International for 

use in compliance monitoring. 

J. Congressional Review Act 

The Congressional Review Act, 5 

U.S.C. Section 801 et seq., as added by 

the Small Business Regulatory 

Enforcement Fairness Act of 1996, 

generally provides that before a rule 

may take effect, the agency 

promulgating the rule must submit a 

rule report, which includes a copy of 

the rule, to each House of the Congress 

and to the Comptroller General of the 

United States. EPA will submit a report 

containing this rule and other required 

information to the U.S. Senate, the U.S. 

House of Representatives, and the 

Comptroller General of the United 

States prior to publication of the rule in 

the Federal Register. A major rule 

cannot take effect until 60 days after it 

is published in the Federal Register. 

This action is not a ‘‘major rule’’ as 

defined by 5 U.S. C Section 804(2). This 

rule will be effective April 11, 2007. 

List of Subjects 

40 CFR Part 122 

Administrative practice and 

procedure, Confidential business 

information, Environmental protection, 

Hazardous substances, Reporting and 

recordkeeping requirements, Water 

pollution control. 

40 CFR Part 136 

Environmental protection, 

Incorporation by reference, Reporting 

and recordkeeping requirements, Water 

pollution control. 

40 CFR Part 141 

Chemicals, Environmental protection, 

Incorporation by reference, Indianslands, Intergovernmental relations, 

Radiation Protection, Reporting and 

recordkeeping requirements, Water 

supply. 

40 CFR Part 143 

Chemicals, Environmental protection, 

Incorporation by reference, Indianslands, Water supply. 

40 CFR Part 430 

Environmental protection, Paper and 

paper products industry, Reporting and 

recordkeeping requirements, Waste 

treatment and disposal, Water pollution 

control. 

40 CFR Part 455 

Chemicals, Environmental protection, 

Packaging and containers, Pesticides 

and pests, Waste treatment and 

disposal, Water pollution control. 


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11211 

40 CFR Part 465 

Coil coating industry, Environmental 

protection, Reporting and recordkeeping 

requirements, Waste treatment and 

disposal, Water pollution control. 

Dated: July 21, 2006. 

Stephen L. Johnson, 

Administrator. 

■ For the reasons set out in the 

preamble, title 40, chapter I of the Code 

of Federal Regulations, is amended as 

follows: 

PART 122—EPA ADMINISTERED 

PERMIT PROGRAMS: THE NATIONAL 

POLLUTANT DISCHARGE 

ELIMINATION SYSTEM 

■ 1. The authority citation for Part 122 

continues to read as follows: 

Authority: The Clean Water Act, 33 U.S.C. 

1251 et seq. 

■ 2. Section 122.1 is amended by 

revising paragraph (a)(4) to read as 

follows: 

§ 122.1 Purpose and Scope. 

(a) * * * 

(4) Regulatory provisions in Parts 125, 

129, 133, 136 of this chapter and 40 CFR 

subchapter N and subchapter O of this 

chapter also implement the NPDES 

permit program. 

* * * * * 

■ 3. Section 122.21 is amended as 

follows: 

■ a. By revising paragraph (g)(7)(i). 

■ b. By revising introductory text in 

paragraph (h)(4)(i). 

■ c. By revising paragraph (j)(4)(viii). 

§ 122.21 Application for a permit 

(applicable to State programs, see § 123.25) 

* * * * * 

(g) * * * 

(7) Effluent characteristics. (i) 

Information on the discharge of 

pollutants specified in this paragraph 

(g)(7) (except information on storm 

water discharges which is to be 

provided as specified in § 122.26). 

When ‘‘quantitative data’’ for a pollutant 

are required, the applicant must collect 

a sample of effluent and analyze it for 

the pollutant in accordance with 

analytical methods approved under Part 

136 of this chapter unless use of another 

method is required for the pollutant 

under 40 CFR subchapters N or O. 

When no analytical method is approved 

under Part 136 or required under 

subchapters N or O, the applicant may 

use any suitable method but must 

provide a description of the method. 

When an applicant has two or more 

outfalls with substantially identical 

effluents, the Director may allow the 

applicant to test only one outfall and 

report that quantitative data as applying 

to the substantially identical outfall. 

The requirements in paragraphs 

(g)(7)(vi) and (vii) of this section state 

that an applicant must provide 

quantitative data for certain pollutants 

known or believed to be present do not 

apply to pollutants present in a 

discharge solely as the result of their 

presence in intake water; however, an 

applicant must report such pollutants as 

present. When paragraph (g)(7) of this 

section requires analysis of pH, 

temperature, cyanide, total phenols, 

residual chlorine, oil and grease, fecal 

coliform (including E. coli), and 

Enterococci (previously known as fecal 

streptococcus at § 122.26 

(d)(2)(iii)(A)(3)), or volatile organics, 

grab samples must be collected for those 

pollutants. For all other pollutants, a 24- 

hour composite sample, using a 

minimum of four (4) grab samples, must 

be used unless specified otherwise at 40 

CFR Part 136. However, a minimum of 

one grab sample may be taken for 

effluents from holding ponds or other 

impoundments with a retention period 

greater than 24 hours. In addition, for 

discharges other than storm water 

discharges, the Director may waive 

composite sampling for any outfall for 

which the applicant demonstrates that 

the use of an automatic sampler is 

infeasible and that the minimum of four 

(4) grab samples will be a representative 

sample of the effluent being discharged. 

Results of analyses of individual grab 

samples for any parameter may be 

averaged to obtain the daily average. 

Grab samples that are not required to be 

analyzed immediately (see Table II at 40 

CFR 136.3 (e)) may be composited in the 

laboratory, provided that container, 

preservation, and holding time 

requirements are met (see Table II at 40 

CFR 136.3 (e)) and that sample integrity 

is not compromised by compositing. 

* * * * * 

(h) * * * 

(4) * * * 

(i) Quantitative data for the pollutants 

or parameters listed below, unless 

testing is waived by the Director. The 

quantitative data may be data collected 

over the past 365 days, if they remain 

representative of current operations, and 

must include maximum daily value, 

average daily value, and number of 

measurements taken. The applicant 

must collect and analyze samples in 

accordance with 40 CFR Part 136. When 

analysis of pH, temperature, residual 

chlorine, oil and grease, or fecal 

coliform (including E. coli), and 

Enterococci (previously known as fecal 

streptococcus) and volatile organics is 

required in paragraphs (h)(4)(i)(A) 

through (K) of this section, grab samples 

must be collected for those pollutants. 

For all other pollutants, a 24-hour 

composite sample, using a minimum of 

four (4) grab samples, must be used 

unless specified otherwise at 40 CFR 

Part 136. For a composite sample, only 

one analysis of the composite of aliquots 

is required. New dischargers must 

include estimates for the pollutants or 

parameters listed below instead of 

actual sampling data, along with the 

source of each estimate. All levels must 

be reported or estimated as 

concentration and as total mass, except 

for flow, pH, and temperature. 

* * * * * 

(j) * * * 

(4) * * * 

(viii) Applicants must collect samples 

of effluent and analyze such samples for 

pollutants in accordance with analytical 

methods approved under 40 CFR Part 

136 unless an alternative is specified in 

the existing NPDES permit. When 

analysis of pH, temperature, cyanide, 

total phenols, residual chlorine, oil and 

grease, fecal coliform (including E. coli), 

or volatile organics is required in 

paragraphs (j)(4)(ii) through (iv) of this 

section, grab samples must be collected 

for those pollutants. For all other 

pollutants, 24-hour composite samples 

must be used. For a composite sample, 

only one analysis of the composite of 

aliquots is required. 

* * * * * 

■ 4. Section 122.41 is amended by 

revising paragraphs (j)(4) and (l)(4)(ii) to 

read as follows: 

§ 122.41 Conditions applicable to all 

permits (applicable to State programs, see 

§ 123.25). 

* * * * * 

(j) * * * 

(4) Monitoring must be conducted 

according to test procedures approved 

under 40 CFR Part 136 unless another 

method is required under 40 CFR 

subchapters N or O. 

* * * * * 

(l) * * * 

(4) * * * 

(ii) If the permittee monitors any 

pollutant more frequently than required 

by the permit using test procedures 

approved under 40 CFR Part 136, or 

another method required for an 

industry-specific waste stream under 40 

CFR subchapters N or O, the results of 

such monitoring shall be included in 

the calculation and reporting of the data 

submitted in the DMR or sludge 

reporting form specified by the Director. 

* * * * * 


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■ 5. Section 122.44 is amended by 

revising paragraph (i)(1)(iv) to read as 

follows: 

§ 122.44 Establishing limitations, 

standards, and other permit conditions 

(applicable to State NPDES programs; see 

§ 123.25). 

* * * * * 

(i) * * * 

(1) * * * 

(iv) According to test procedures 

approved under 40 CFR Part 136 for the 

analyses of pollutants or another 

method is required under 40 CFR 

subchapters N or O. In the case of 

pollutants for which there are no 

approved methods under 40 CFR Part 

136 or otherwise required under 40 CFR 

subchapters N or O, monitoring must be 

conducted according to a test procedure 

specified in the permit for such 

pollutants. 

* * * * * 

PART 136—GUIDELINES 

ESTABLISHING TEST PROCEDURES 

FOR THE ANALYSIS OF POLLUTANTS 

■ 6. 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.) 

■ 7. Section 136.3 is amended as 

follows: 

■ a. In paragraph (a) by revising the 

introductory text and Tables IA, IB, IC, 

ID, and IE. 

■ b. In paragraph (a) by adding Table IG 

after the notes of Table IF. 

■ c. In paragraph (b) by revising 

references 6, 10, and 17, and adding 

references 63 through 69. 

■ d. By revising paragraphs (c), (d), and 

(e). 

§ 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, and IG. In the event 

of a conflict between the reporting 

requirements of 40 CFR Parts 122 and 

125 and any reporting requirements 

associated with the methods listed in 

these tables, the provisions of 40 CFR 

Parts 122 and 125 are controlling and 

will determine a permittee’s reporting 

requirements. The full text of the 

referenced test procedures are 

incorporated by reference into Tables 

IA, IB, IC, ID, IE, IF, and IG. The 

incorporation by reference of these 

documents, as specified in paragraph (b) 

of this section, was approved by the 

Director of the Federal Register in 

accordance with 5 U.S.C. 552(a) and 1 

CFR Part 51. Copies of the documents 

may be obtained from the sources listed 

in paragraph (b) of this section. You can 

get information about obtaining these 

documents from the EPA Office of 

Water Engineering and Analysis 

Division at 202–566–1000. Documents 

may be inspected at EPA’s Water 

Docket, EPA West, 1301 Constitution 

Avenue, NW., Washington, DC 

(Telephone: 202–566–2426); or at the 

National Archives and Records 

Administration (NARA). For 

information on the availability of this 

material at NARA, call 202–741–6030, 

or go to: http://www.archives.gov/

federal_register/code_of_federal_

regulations/ibr_locations.html 

These test procedures are 

incorporated as they exist on the day of 

approval and a notice of any change in 

these test procedures will be published 

in the Federal Register. The discharge 

parameter values for which reports are 

required must be determined by one of 

the standard analytical test procedures 

incorporated by reference and described 

in Tables IA, IB, IC, IE, IF, and IG 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 

(b) or (c) of this section or 40 CFR 

401.13) other test procedures may be 

used if such other test procedures have 

been previously approved by the 

Regional Administrator of the Region in 

which the discharge will occur, and the 

Director of the State in which such 

discharge will occur does not object to 

the use of an additional or alternate test 

procedure. 

TABLE IA.—LIST OF APPROVED BIOLOGICAL METHODS

Parameter and units Method 1 EPA 

Standard 

methods 18th, 

19th, 20th Ed. 

Standard 

methods online 

AOAC, 

ASTM, 

USGS 

Other 

Bacteria: 

1. Coliform (fecal), 

number per 100 

mL.

Most Probable Number 

(MPN), 5 tube 3 dilution, or 

p. 132 3 ............. 9221C or E ....... 9221C or E–99.

Membrane filter (MF) 2, 

single step.

p. 124 3 ............. 9222D ............... 9222D–97 ........... B–0050– 

85 5.

2. Coliform (fecal) in 

presence of chlorine, number per 

100 mL.

MPN, 5 tube, 3 dilution, 

or 

p. 132 3 ............. 9221C or E ....... 9221C or E–99.

MF, single step 6 ........... p. 124 3 ............. 9222D ............... 9222D–97.

3. Coliform (total), 

number per 100 

mL.

MPN, 5 tube, 3 dilution, 

or 

p. 114 3 ............. 9221B ............... 9221B–99.

MF 2, single step or two 

step.

p. 108 3 ............. 9222B ............... 9222B–97 ........... B–0025– 

85 5.

4. Coliform (total), 

in presence of 

chlorine, number 

per 100 mL.

MPN, 5 tube, 3 dilution, 

or 

p. 114 3 ............. 9221B ............... 9221B–99.

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

97.

5. E. coli, number 

per 100 mL 28.

MPN 7, 9, 15, multiple 

tube, 

........................... 9221B.1/ 

9221F12 14.

9221B.1–99/ 

9221F12 14.


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11213 

TABLE IA.—LIST OF APPROVED BIOLOGICAL METHODS—Continued 

Parameter and units Method 1 EPA 

Standard 

methods 18th, 

19th, 20th Ed. 

Standard 

methods online 

AOAC, 

ASTM, 

USGS 

Other 

multiple tube/multiple 

well, 

........................... 9223B13 ........... 9223B–97 13 ....... 991.15 11 .... Colilert 13, 17, 

Colilert18 13, 16, 17

MF two step, or ............. 1103.1 20 ........... 9222B/9222G 19, 

9213D.

9222B–97/ 

9222G 19.

D5392–

93 10.

single step ..................... 1603 21, 1604 22 ........................... ............................ ................... mColiBlue-24 18

6. Fecal 

streptococci, 

number per 100 

mL.

MPN, 5 tube, 3 dilution, p. 139 3 ............. 9230B ............... 9230B–93.

MF 2, or ......................... p. 136 3 ............. 9230C ............... 9230C–93 ........... B–0055–

85 5.

Plate count .................... p. 143 3.

7. Enterococci, 

number per 100 

mL 28.

MPN 7, 9 multiple tube, .. ........................... 9230B ............... 9230B–93.

multiple tube/multiple 

well.

........................... ........................... ............................ D6503–

99 10.

Entero-lert 13, 23

MF 2, 6, 7, 8, 9, two step ...

single step, or ...............

Plate count ....................

1106.1 24 ...........

1600 25. 

p. 143 3. 

9230C ............... 9230C–93 ........... D5259–

92 10.

Protozoa: 

8. Cryptosporidium 28.Filtration/IMS/FA ........... 1622 26, 1623 27.

9. Giardia 28 ............ Filtration/IMS/FA ........... 1623 27.

Aquatic Toxicity: 

10. Toxicity, acute, 

fresh water organisms, LC50, percent effluent.

Ceriodaphnia dubia 

acute.

2002.0 29.

Daphnia puplex and 

Daphnia magna acute.

2021.0 29.

Fathead Minnow, 

Pimephales promelas, 

and Bannerfin shiner, 

Cyprinella leedsi, 

acute.

2000.0 29.

Rainbow Trout, 

Oncorhynchus 

mykiss, and brook 

trout, Salvelinus 

fontinalis, acute.

2019.0 29.

11. Toxicity, acute, 

estuarine and 

marine organisms 

of the Atlantic 

Ocean and Gulf 

of Mexico, LC50, 

percent effluent.

Mysid, Mysidopsis 

bahia, acute.

2007.0 29.

Sheepshead Minnow, 

Cyprinodon 

variegatus, acute.

2004.0 29.

Silverside, Menidia 

beryllina, Menidia 

menidia, and Menidia 

peninsulae, acute.

2006.0 29.

12. Toxicity, chronic, fresh water organisms, NOEC 

or IC25, percent 

effluent.

Fathead minnow, 

Pimephales promelas, 

larval survival and 

growth.

1000.0 30.

Fathead minnow, 

Pimephales promelas, 

embryo-larval survival 

and teratogenicity.

1001.0 30.

Daphnia, Ceriodaphnia 

dubia, survival and reproduction.

1002.0 30.


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11214 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IA.—LIST OF APPROVED BIOLOGICAL METHODS—Continued 

Parameter and units Method 1 EPA 

Standard 

methods 18th, 

19th, 20th Ed. 

Standard 

methods online 

AOAC, 

ASTM, 

USGS 

Other 

Green alga, 

Selenastrum 

capricornutum, growth.

1003.0 30.

13. Toxicity, chronic, estuarine and 

marine organisms 

of the Atlantic 

Ocean and Gulf 

of Mexico, NOEC 

or IC25, percent 

effluent.

Sheepshead minnow, 

Cyprinodon 

variegatus, larval survival and growth.

1004.0 31.

Sheepshead minnow, 

Cyprinodon 

variegatus, embryolarval survival and 

teratogenicity.

1005.0 31.

Inland silverside, 

Menidia beryllina, larval survival and 

growth.

1006.0 31.

Mysid, Mysidopsis 

bahia, survival, 

growth, and fecundity.

1007.0 31.

Sea urchin, Arbacia 

punctulata, fertilization.

1008.0 31.

1The method must be specified when results are reported. 

2A 0.45-μ membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of 

extractables which could interfere with their growth. 3 USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati, OH, EPA/600/8–78/017. 4 [Reserved] 

5 USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for 

Collection and Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of Interior, Reston, VA. 6Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be 

required to resolve any controversies. 7Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample. 8When the MF method has not been used previously to test ambient waters with high turbidity, large number of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results. 9To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons 

of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and 

Wastewater or EPA alternate test procedure (ATP) guidelines. 10ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. ASTM International. 100 

Barr Harbor Drive, West Conshohocken, PA 19428. 11AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical 

Chemists International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877–2417. 12The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel 

tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase 

on 10 percent of all total coliform-positive tubes on a seasonal basis. 13These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme b-glucuronidase produced by E. coli. 14After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of 

gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F. Commercially available EC–MUG media or EC media supplemented in the laboratory with 50 μg/mL of MUG may be used. 15Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube 

and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert may be enumerated with the multiple-well procedures, Quanti-Tray or Quanti-Tray 2000, and the MPN calculated from the table provided by the manufacturer. 16 Colilert-18 is an optimized formulation of the Colilert for the determination of total coliforms and E. coli that provides results within 18 h of 

incubation at 35 °C rather than the 24 h required for the Colilert test and is recommended for marine water samples. 17 Descriptions of the Colilert, Colilert-18, Quanti-Tray, and Quanti-Tray/2000 may be obtained from IDEXX Laboratories, Inc., 1 IDEXX 

Drive, Westbrook, ME 04092. 18A description of the mColiBlue24 test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010. 19Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA MUG media. 20 USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) In Water By Membrane Filtration Using membrane-Thermotolerant Escherichia coli 

Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–02–020. 21 USEPA. 2002. Method 1603: Escherichia coli (E. coli) In Water By Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar ( modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–02–023. 22Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ‘‘New Medium for 

the Simultaneous Detection of Total Coliform and Escherichia coli in Water.’’ Appl. Environ. Microbiol. 59:3534–3544 and in USEPA. 2002. Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA 821–R–02–024. 23A description of the Enterolert test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092. 


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11215 

24 USEPA. 2002. Method 1106.1: Enterococci In Water By Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE–EIA). 

U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–02–021. 25 USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b-D-Glucoside Agar 

(mEI). U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–02–022. 26 Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of 

Cryptosporidium. USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of 

Water, Washington, DC, EPA–821–R–01–026. 27 Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence 

assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA–821–R–01–025. 28 Recommended for enumeration of target organism in ambient water only. 29 USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. 

Fifth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R–02/012. 30 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. 

Fourth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC, EPA/821/R–02/013. 31 USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine 

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


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11216 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IB.

—

LIST OF

APPROVED INORGANIC

TEST

PROCEDURES

Parameter Methodology 58

Reference (method number or page) 

EPA35, 52 Standard methods (18th, 19th) Standard methods (20th) Standard methods online ASTM USGS/AOAC/other 

1. Acidity, as CaCO3, mg/L ............................ Electrometric endpoint or phenolphthalein endpoint. ............................... 2310 B(4a) ........... 2310 B(4a) ........... 2310 B(4a)–97 ........ D1067–92, 02 ....... I–1020–85 22. Alkalinity, as CaCO3, mg/L ......................... Electrometric or Colorimetric titration 

to pH 4.5, manual, or 

............................... 2320 B .................. 2320 B .................. 2320 B–97 .............. D1067–92, 02 ....... 973.43 3, I–1030–

85 2

automatic ............................................ 310.2 (Rev. 

1974) 1.

............................... ............................... ................................. ............................... I–2030–85 2

3. Aluminum

—Total,4 mg/L ............................ Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 D .................. ............................... 3111 D–99 .............. ............................... I–3051–85 2AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99.STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–9750 

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.143

Direct Current Plasma (DCP) 36 ......... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Eriochrome cyanine R) ............................... 3500–Al D ............ 3500–Al B ............. 3500–Al B–01.

4. Ammonia (as N), mg/L ............................... Manual, distillation (at pH 9.5) 6 followed by: 350.1, Rev. 2.0 (1993). 4500–NH B3 ......... 4500–NH3 B ......... 4500–NH3 B–97 ...... ............................... 973.49 3

Nesslerization ..................................... ............................... 4500–NH3 C (18th 

only).

............................... ................................. D1426–98, 03 (A) 973.49 3, I–3520–

85 2

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

(19th) and 4500–NH3 E 

(18th).

4500–NH3 C ......... 4500–NH3 C–97.

Electrode ............................................ ............................... 4500–NH3 D or E 

(19th) and 4500–NH3 F or 

G (18th).

4500–NH3 D or E 4500–NH3 D or E–

97.

D1426–98, 03 (B).

Automated phenate, or ...................... 350.1 60, Rev. 2.0 

(1993).

4500–NH3 G 

(19th) and 4500–NH3 H 

(18th).

4500–NH3 G ......... 4500–NH3 G–97 ..... ............................... I–4523–85 2

Automated electrode .......................... ............................... ............................... ............................... ................................. ............................... See footnote 7 Ion Chromatography .......................... ............................... ............................... ............................... ................................. D6919–03.

5. Antimony

—Total, 4 mg/L ............................. Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99.STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

6. Arsenic

—Total, 4 mg/L ............................... Digestion 4 followed by ....................... 206.5 (Issued 

1978) 1.

AA gaseous hydride ........................... ............................... 3114 B 4.d ............ ............................... 3114 B 4.d–97 ........ D2972–97, 03 (B) I–3062–85 2AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D2972–97, 03 (C) I–4063–98 49STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

Colorimetric (SDDC) .......................... ............................... 3500–As C ........... 3500–As B ............ 3500–As B–97 ........ D2972–97, 03 (A) I–3060–85 

7. Barium

—Total,4 mg/L ................................. Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 D .................. ............................... 3111 D–99 .............. ............................... I–3084–85 2AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D4382–95, 02.


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11217 

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

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

8. Beryllium

—Total,4 mg/L .............................. Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 D .................. ............................... 3111 D–99 .............. D3645–93 (88), 03 

(A).

I–3095–85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D3645–93 (88), 03 

(B).

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

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP, or .............................................. ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (aluminon) ...................... ............................... 3500–Be D.

9. Biochemical oxygen demand (BOD5), mg/ 

L.

Dissolved Oxygen Depletion .............. ............................... 5210 B .................. 5210 B .................. 5210 B–01 .............. ............................... 973.44,3 p. 17.9, I–

1578–78 8

10. Boron

—Total,37 mg/L ............................... Colorimetric (curcumin) ...................... ............................... 4500–B B ............. 4500–B B ............. 4500–B B–00 .......... ............................... I–3112–85 2

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

(1994).

3120 B .................. 3120 B .................. 3120 B 99 ................ ............................... I–4471–97 50

DCP .................................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34 

11. Bromide, mg/L .......................................... Titrimetric ........................................... ............................... ............................... ............................... ................................. D1246–95, 99 (C) p. S44.10

............................................................ ............................... ............................... ............................... ................................. ............................... I–1125–85 2

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

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

12. Cadmium

—Total,4 mg/L ........................... Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D3557–95, 02 (A 

or B).

974.27,3 p. 37.9, I–

3135–85 2 or I–

3136–85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D3557–95, 02 (D) I–4138–89 51STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–1472–852 or I–

4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP36 ................................................ ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Voltametry 11, or ................................. ............................... ............................... ............................... ................................. D3557–95, 02 (C).Colorimetric (Dithizone) ..................... ............................... 3500–Cd D.

13. Calcium

—Total,4 mg/L ............................. Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99 .............. D511–93, 03(B) .... I–3152–85 2ICP/AES ............................................. 200.7, Rev. 4.4 

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

DCP, or .............................................. ............................... ............................... ............................... ................................. ............................... See footnote 34Titrimetric (EDTA) .............................. ............................... 3500–Ca D ........... 3500–Ca B ........... 3500–Ca B–97 ........ D511–93, 03(A).Ion Chromatography .......................... ............................... ............................... ............................... ................................. D6919–03.

14. Carbonaceous biochemical oxygen demand (CBOD5), mg/L 12. Dissolved Oxygen Depletion with ni- trification inhibitor. ............................... 5210 B .................. 5210 B .................. 5210 B–01.15. Chemical oxygen demand (COD), mg/L .. Titrimetric ........................................... 410.3 (Rev. 

1978) 1.

5220 C .................. 5220 C .................. 5220 C–97 .............. D1252–95, 00 (A) 973.46 3, p. 17 9 I–

3560–85 2

Spectrophotometric, manual or automatic. 410.4, Rev. 2.0 (1993). 5220 D .................. 5220 D .................. 5220 D–97 .............. D1252–95, 00 (B) See foot- notes 13, 14. I–

3561–85 2

16. Chloride, mg/L .......................................... Titrimetric: (silver nitrate) or ............... ............................... 4500–Cl–B ............ 4500–Cl–B ............ 4500–Cl–B–97 ........ D512–89(99) (B) .. I–1183–85 2

(Mercuric nitrate) ................................ ............................... 4500–Cl–C ........... 4500–Cl–C ........... 4500–Cl–C–97 ........ D512–89 (99) (A) 973.51 3, I–1184–

85 2

Colorimetric: manual or ...................... ............................... ............................... ............................... ................................. ............................... I–1187–85 2Automated (Ferricyanide) .................. ............................... 4500–Cl–E ............ 4500–Cl–E ............ 4500–Cl–E–97 ........ ............................... I–2187–85 2Potentiometric Titration ...................... ............................... 4500–Cl–D ........... 4500–Cl–D ........... 4500–Cl–D–97.Ion Selective Electrode ...................... ............................... ............................... ............................... ................................. D512–89(99)(C).


rwilkins on PROD1PC63 with RULES
11218 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IB.

—

LIST OF

APPROVED INORGANIC

TEST

PROCEDURES

—Continued 

Parameter Methodology 58

Reference (method number or page) 

EPA35, 52 Standard methods (18th, 19th) Standard methods (20th) Standard methods online ASTM USGS/AOAC/other 

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

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

17. Chlorine

—Total residual, mg/L; Titrimetric Amperometric direct, or ..................... ............................... 4500–Cl D ............ 4500–Cl D ............ 4500–Cl D–00 ......... D1253–86 (96), 03.

Amperometric direct (low level) ......... ............................... 4500–Cl E ............ 4500–Cl E ............ 4500–Cl E–00.Iodometric direct ................................ ............................... 4500–Cl B ............ 4500–Cl B ............ 4500–Cl B–00.Back titration ether end–point 15 or .... ............................... 4500–Cl C ............ 4500–Cl C ............ 4500–Cl C–00.DPD–FAS ........................................... ............................... 4500–Cl F ............. 4500–Cl F ............. 4500–Cl F–00.Spectrophotometric, DPD or .............. ............................... 4500–Cl G ............ 4500–Cl G ............ 4500–Cl G–00.Electrode ............................................ ............................... ............................... ............................... ................................. ............................... See footnote 16

18. Chromium VI dissolved, mg/L .................. 0.45–micron Filtration followed by: 

AA chelation–extraction or ................. ............................... 3111 C .................. ............................... 3111 C–99 .............. ............................... I–1232–85 Ion Chromatography .......................... 218.6, Rev. 3.3 

(1994).

3500–Cr E ............ 3500–Cr C ............ 3500–Cr C–01 ........ D5257–97 ............. 993.23 

Colorimetric (Diphenyl–carbazide) ..... ............................... 3500–Cr D ............ 3500–Cr B ............ 3500–Cr B–01 ......... D1687–92, 02 (A) I–1230–85 

19. Chromium

—Total,4 mg/L .......................... Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B .................. ............................... 3111 B–99 .............. D1687–92, 02 (B) 974.27 3, I–3236–

85 2

AA chelation–extraction ..................... ............................... 3111 C .................. ............................... 3111 C–99.AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D1687–92, 02 (C) I–3233–93 46STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP,36 or ........................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Diphenyl–carbazide) ..... ............................... 3500–Cr D ............ 3500–Cr B ............ 3500–Cr B–01.

20. Cobalt

—Total,4 mg/L ................................ Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D3558–94, 03 (A 

or B).

p. 37 9, I–3239–

85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D3558–94, 03 (C) I–4243–89 51STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP .................................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34

21. Color, platinum cobalt units or dominant 

wavelength, hue, luminance purity.

Colorimetric (ADMI), or ...................... ............................... 2120 E .................. 2120 E .................. ................................. ............................... See footnote 18

(Platinum cobalt), or ........................... ............................... 2120 B .................. 2120 B .................. 2120 B–01 .............. ............................... I–1250–85 2Spectrophotometric ............................ ............................... 2120 C .................. 2120 C.

22. Copper

—Total,4 mg/L ............................... Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D1688–95, 02 (A 

or B).

974.27 3 p. 37 9 I–

3270–85 2 or I–

3271–85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D1688–95, 02 (C) I–4274–89 51STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP36 or ........................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Neocuproine) or ............ ............................... 3500–Cu D ........... 3500–Cu B ........... 3500–Cu B–99.(Bicinchoninate) ................................. ............................... 3500–Cu E ........... 3500–Cu C ........... 3500–Cu C–99 ........ ............................... See footnote 19


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11219 

23. Cyanide

—Total, mg/L ............................... Automated Distillation and Colorimetry, or. ............................... ............................... ............................... ................................. ............................... Kelada–01 55

Manual distillation with MgCl2 followed by: 335.4, Rev. 1.0 (1993) 57. 4500–CN–C .......... 4500–CN–C .......... ................................. D2036–98(A) ........ 10–204–00–1–X56Titrimetric or ....................................... ............................... 4500–CN–D .......... 4500–CN–D .......... 4500–CN–D–99 ....... ............................... p. 22 9Spectrophotometric, manual or .......... ............................... 4500–CN–E .......... 4500–CN–E .......... 4500–CN–E–99 ....... D2036–98(A) ........ I–3300–85 Automated 20 or .................................. 335.4, Rev. 1.0 

(1993) 57.

............................... ............................... ................................. ............................... 10–204–00–1–X56, 

I–4302–85 2

Ion Selective Electrode ...................... ............................... 4500–CN–F ........... 4500–CN–F ........... 4500–CN–F–99 ....... D2036–98(A).

24. Available Cyanide, mg/L .......................... Cyanide Amenable to Chlorination 

(CATC); Manual distillation with MgCl2 followed by Titrimetric or 

Spectrophotometric.

............................... 4500–CN–G .......... 4500–CN–G .......... 4500–CN–G–99 ....... D2036–98(B).

Flow injection and ligand exchange, 

followed by amperometry 61.

............................... ............................... ............................... ................................. D6888–04 ............. OIA–1677 44

Automated Distillation and Colorimetry. ............................... ............................... ............................... ................................. ............................... Kelada–01 55

25. Fluoride

—Total, mg/L ............................... Manual distillation6 followed by: ............................... 4500–F–B ............. 4500–F–B ............. 4500–F–B–97.

Electrode, manual or .......................... ............................... 4500–F–B ............. 4500–F–B ............. 4500–F–C–97 .......... D1179–93, 99 (B).Automated .......................................... ............................... ............................... ............................... ................................. ............................... I–4327–85 2Colorimetric, (SPADNS) or ................ ............................... 4500–F–D ............. 4500–F–D ............. 4500–F–D–97 .......... D1179–93, 99 (A).Automated complexone ..................... ............................... 4500–F–E ............. 4500–F–E ............. 4500–F–E–97.Ion Chromatography .......................... 300.0, Rev 2.1 

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97,03 ........ 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

26. Gold

—Total,4 mg/L ................................... Digestion 4 followed by: 

AA direct aspiration, or ...................... ............................... 3111 B .................. ............................... 3111 B–99.AA furnace, or .................................... 231.2 (Rev. 

1978) 1.

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

27. Hardness

—Total, as CaCO3, mg/L .......... Automated colorimetric, ..................... 130.1 (Issued 

1971) 1.

Titrimetric (EDTA) or .......................... ............................... 2340 B or C .......... 2340 B or C .......... 2340 B or C–97 ...... D1126–86(92), 02 973.5 2B3, I–

1338–852

Ca plus Mg as their carbonates, by 

inductively coupled plasma or AA direct aspiration. (See Parameters 13 and 33)..

28. Hydrogen ion (pH), pH units .................... Electrometric measurement or ........... ............................... 4500–H∂ B .......... 4500–H∂ B .......... 4500–H∂ B–00 ....... D1293–84 (90), 99 

(A or B).

973.41.3, I–1586–

85 2

Automated electrode .......................... 150.2 (Dec. 

1982) 1.

............................... ............................... ................................. ............................... See footnote21, I–

2587–852

29. Iridium

—Total,4 mg/L ................................ Digestion 4 followed by: 

AA direct aspiration or ....................... ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... 235.2 (Issued 

1978) 1.

30. Iron

—Total,4 mg/L .................................... Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D1068–96, 03 (A 

or B).

974.27 3, I–3381–

85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D1068–96, 03 (C).STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

DCP36 or ........................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Phenanthroline) ............ ............................... 3500–Fe D ........... 3500–Fe B ............ 3500–Fe B–97 ........ D1068–96, 03 (D) See footnote 22

31. Kjeldahl Nitrogen 5—Total, (as N), mg/L .. Digestion and distillation followed 

by: 20

............................... 4500–Norg B or C 

and 4500–NH3

B.

4500–Norg B or C 

and 4500–NH3

B.

4500–Norg B or C–

97 and 4500–NH3

B–97.

D3590–89, 02 (A).

Titration or .......................................... ............................... 4500–NH3 C 

(19th) and 4500–NH 3 E 

(18th).

4500–NH3 C ......... 4500–NH3 C–97 ..... D3590–89, 02 (A) 973.48 3


rwilkins on PROD1PC63 with RULES
11220 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IB.

—

LIST OF

APPROVED INORGANIC

TEST

PROCEDURES

—Continued 

Parameter Methodology 58

Reference (method number or page) 

EPA35, 52 Standard methods (18th, 19th) Standard methods (20th) Standard methods online ASTM USGS/AOAC/other 

Nesslerization or ................................ ............................... 4500–NH3 C (18th 

Only).

............................... ................................. D3590–89, 02 (A).

Electrode ............................................ ............................... 4500–NH3 F or G 

(18th) and 4500–NH3 D or 

E (19th).

4500–NH3 D or E 4500–NH3 D or E–

97.

Automated phenate colorimetric ........ 351.1 (Rev. 

1978) 1.

............................... ............................... ................................. ............................... I–4551–78 8

Semi-automated block digestor colorimetric. 351.2, Rev. 2.0 (1993). ............................... ............................... ................................. D3590–89, 02 (B) I–4515–91 45Manual or block digestor potentiometric. ............................... ............................... ............................... ................................. D3590–89, 02 (A).Block digester, followed by Auto distillation and Titration, or. ............................... ............................... ............................... ................................. ............................... See footnote 39Nesslerization, or ............................... ............................... ............................... ............................... ................................. ............................... See footnote 40Flow injection gas diffusion ................ ............................... ............................... ............................... ................................. ............................... See footnote 41

32. Lead

—Total,4 mg/L .................................. Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D3559–96, 03 (A 

or B).

974.27 3, I–3399–

85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D3559–96, 03 (D) I–4403–89 51STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP36 ................................................ ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Voltametry 11 or .................................. ............................... ............................... ............................... ................................. D3559–96, 03 (C).Colorimetric (Dithizone) ..................... ............................... 3500–Pb D ........... 3500–Pb B ........... 3500–Pb B–97.

33. Magnesium

—Total,4 mg/L ........................ Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99 .............. D511–93, 03(B) .... 974.27 3, I–3447–

85 2

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

DCP or ............................................... ............................... ............................... ............................... ................................. ............................... See footnote 34Gravimetric ......................................... ............................... 3500–Mg D.Ion Chromatography .......................... ............................... ............................... ............................... ................................. D6919–03.

34. Manganese

—Total,4 mg/L ........................ Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B .................. ............................... 3111 B–99 .............. D858–95, 02 (A or 

B).

974.27 3, I–3454–

85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D858–95, 02 (C).STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP36, or .......................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Persulfate), or ............... ............................... 3500––Mn D ......... 3500–Mn B ........... 3500–Mn B–99 ....... ............................... 920.203 3(Periodate) ......................................... ............................... ............................... ............................... ................................. ............................... See footnote 23

35. Mercury

—Total 4, mg/L ............................. Cold vapor, manual or ....................... 245.1, Rev. 3.0 

(1994).

3112 B .................. ............................... 3112 B–99 .............. D3223–97, 02 ....... 977.22 3, I–3462–

852

Automated .......................................... 245.2 (Issued 

1974).

Cold vapor atomic fluorescence 

spectrometry (CVAFS).

245.7 Rev. 2.0 

(2005) 59.

Purge and Trap CVAFS ..................... 1631E43.

36. Molybdenum

—Total 4, mg/L ..................... Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 D .................. ............................... 3111 D–99 .............. ............................... I–3490–85 2


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11221 

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. ............................... I–3492–96 47ICP/AES ............................................. 200.7, Rev. 4.4 

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

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

37. Nickel

—Total,4 mg/L ................................. Digestion 4 followed by: 

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D1886–90, 94 (98) 

(A or B).

I–3499–85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D1886–90, 94 (98) 

(C).

I–4503–89 51

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

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP36, or .......................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (heptoxime) .................... ............................... 3500–Ni D (17th 

Edition).

38. Nitrate (as N), mg/L .................................. Ion Chromatography .......................... 300.0, Rev 2.1 

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54Ion Selective Electrode ...................... ............................... 4500–NO3 –D ....... 4500–NO3 –D ....... 4500–NO3 –D–00.Colorimetric (Brucine sulfate), or ....... 352.1 1 .................. ............................... ............................... ................................. ............................... 973.50 3, 419D 1, 7, 

p. 28 9

Nitrate-nitrite N minus Nitrite N (See 

parameters 39 and 40)..

39. Nitrate-nitrite (as N), mg/L ........................ Cadmium reduction, manual or ......... ............................... 4500–NO3

–E ......... 4500–NO3

–E ......... 4500–NO3–E–00 ..... D3867–99(B).

Automated, or .................................... 353.2, Rev. 2.0 

(1993).

4500–NO3

–F ......... 4500–NO3

–F ......... 4500–NO3

–F–00 ..... D3867–99(A) ........ I–4545–85 2

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

–H ........ 4500–NO3

–H ........ 4500–NO3

–H–00.

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

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97 ............. 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

40. Nitrite (as N), mg/L ................................... Spectrophotometric: Manual or .......... ............................... 4500–NO2

–B ......... 4500–NO2

–B ......... 4500–NO2

–B–00 ..... ............................... See footnote 25

Automated (Diazotization) .................. ............................... ............................... ............................... ................................. ............................... I–4540–85 2Automated (*bypass cadmium reduction). 353.2, Rev. 2.0 (1993). 4500–NO3

–F ......... 4500–NO3

–F ......... 4500–NO3

–F–00 ..... D3867–99(A) ........ I–4545–85 2

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

–E ......... 4500–NO3

–E ......... 4500–NO3

–E–00 ..... D3867–99(B).

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

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev.2 54

41. Oil and grease

—Total recoverable, mg/L Hexane extractable material (HEM): 

n–Hexane extraction and gravimetry.

1664A42 ............... ............................... 5520 B38 .............. 5520 B–01 38.

Silica gel treated HEM (SGT–HEM): 

Silica gel treatment and gravimetry..

1664A42.

42. Organic carbon

—Total (TOC), mg/L ........ Combustion or oxidation .................... ............................... 5310 B, C, or D .... 5310 B, C, or D .... 5310 B, C, or D–00 D2579–93 (A or B) 973.47,3 p. 14 24

43. Organic nitrogen (as N), mg/L ................. Total Kjeldahl N (Parameter 31) 

minus ammonia N (Parameter 4).

44. Orthophosphate (as P), mg/L ................... Ascorbic acid method:.

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

(1993).

4500–P F .............. 4500–P F .............. ................................. ............................... 973.56 3, I–4601–

85 2

Manual single reagent ....................... ............................... 4500–P E ............. 4500–P E ............. ................................. D515–88(A) .......... 973.55 3Manual two reagent ........................... 365.3 (Issued 

1978)1.


rwilkins on PROD1PC63 with RULES
11222 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IB.

—

LIST OF

APPROVED INORGANIC

TEST

PROCEDURES

—Continued 

Parameter Methodology 58

Reference (method number or page) 

EPA35, 52 Standard methods (18th, 19th) Standard methods (20th) Standard methods online ASTM USGS/AOAC/other 

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

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

45. Osmium

—Total 4, mg/L ............................ Digestion 4 followed by: 

AA direct aspiration, or ...................... ............................... 3111 D .................. ............................... 3111 D–99.AA furnace ......................................... 252.2 (Issued 

1978) 1.

46. Oxygen, dissolved, mg/L .......................... Winkler (Azide modification), or ......... ............................... 4500–O C ............. 4500–O C ............. 4500–O C–01 ......... D888–92, 03 (A) ... 973.4 5B3, I–

1575–78 8

Electrode ............................................ ............................... 4500–O G ............. 4500–O G ............. 4500–O G–01 ......... D888–92, 03 (B) ... I–1576–78 8

47. Palladium

—Total,4 mg/L ........................... Digestion 4 followed by: 

AA direct aspiration, or ...................... ............................... 3111 B .................. ............................... 3111 B–99 .............. ............................... p. S27 10AA furnace ......................................... 253.2 1 (Issued 

1978).

............................... ............................... ................................. ............................... p. S28 10

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

48. Phenols, mg/L .......................................... Manual distillation 26 Followed by: 420.1 1 (Rev. 

1978).

............................... ............................... ................................. ............................... See footnote 27

Colorimetric (4AAP) manual, or ......... 420.1 1 (Rev. 

1978).

............................... ............................... ................................. ............................... See footnote 27

Automated .......................................... 420.4 Rev. 1.0 

(1993).

49. Phosphorus (elemental), mg/L ................. Gas–liquid chromatography ............... ............................... ............................... ............................... ................................. ............................... See footnote 2850. Phosphorus

—Total, mg/L ......................... Persulfate digestion followed by: 20 ............................... 4500–P B.5 .......... 4500–P B.5 .......... ................................. ............................... 973.55 3

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

1978).

4500–P E ............. 4500–P E ............. ................................. D515–88(A).

Automated ascorbic acid reduction ... 365.1 Rev. 2.0 

(1993).

4500–P F .............. 4500–P F .............. ................................. ............................... 973.56 3, I–4600–

85 2

Semi–automated block digestor ........ 365.4 1 (Issued 

1974).

............................... ............................... ................................. D515–88(B) .......... I–4610–91 48

51. Platinum

—Total,4 mg/L ............................ Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... 255.2 1.DCP .................................................... ............................... ............................... ............................... ................................. ............................... See footnote 34

52. Potassium

—Total,4 mg/L .......................... Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99 .............. ............................... 973.53 3, I–3630–

85 2

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

Flame photometric, or ........................ ............................... 3500–K D ............. 3500–K B ............. 3500–K B–97.Colorimetric ........................................ ............................... ............................... ............................... ................................. ............................... 317 B17Ion Chromatography .......................... ............................... ............................... ............................... ................................. D6919–03.

53. Residue

—Total, mg/L ............................... Gravimetric, 103–105° ....................... ............................... 2540 B .................. 2540 B .................. 2540 B–97 .............. ............................... I–3750–85 2

54. Residue

—filterable, mg/L ......................... Gravimetric, 180° ............................... ............................... 2540 C .................. 2540 C .................. 2540 C–97 .............. ............................... I–1750–85 2

55. Residue

—non–filterable (TSS), mg/L ...... Gravimetric, 103–105 °C post washing of residue. ............................... 2540 D .................. 2540 D .................. 2540 D–97 .............. ............................... I–3765–85 2

56. Residue

—settleable, mg/L ....................... Volumetric, (Imhoff cone), or 

gravimetric.

............................... 2540 F .................. 2540 F .................. 2540 F–97.

57. Residue

—Volatile, mg/L ........................... Gravimetric, 550 °C ........................... 160.4 1 .................. ............................... ............................... ................................. ............................... I–3753–85 2

58. Rhodium

—Total,4 mg/L ............................ Digestion 4 followed by: 

AA direct aspiration, or ...................... ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... 265.2 1.

59. Ruthenium

—Total,4 mg/L ......................... Digestion 4 followed by: 

AA direct aspiration, or ...................... ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... 267.2 1.

60. Selenium

—Total,4 mg/L ........................... Digestion 4 followed by: 

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. D3859–98, 03 (B) I–4668–98 49


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

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

AA gaseous hydride ........................... ............................... 3114 B .................. ............................... 3114 B–97 .............. D3859–98, 03 (A) I–3667–85 2

61. Silica

—Dissolved,37 mg/L ......................... 0.45 micron filtration followed by: 

Colorimetric, Manual or ...................... ............................... 4500–Si D ............ 4500–SiO2 C ........ 4500–SiO2C–97 ...... D859–94, 00 ......... I–1700–85 2Automated (Molybdosilicate), or ........ ............................... ............................... ............................... ................................. ............................... I–2700–85 2ICP/AES ............................................. 200.7, Rev. 4.4 

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

62. Silver

—Total,4, 31 mg/L ............................. Digestion 4, 29 followed by: 

AA direct aspiration ............................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... ............................... 974.27 3, p. 37 9, I–

3720–85 2

AA furnace ......................................... ............................... 3113 B .................. ............................... 3113 B–99 .............. ............................... I–4724–89 51STGFAA ............................................. 200.9, Rev. 2.2 

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

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

63. Sodium

—Total,4 mg/L .............................. Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99 .............. ............................... 973.54 3, I–3735–

85 2

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

DCP, or .............................................. ............................... ............................... ............................... ................................. ............................... See footnote 34Flame photometric ............................. ............................... 3500–Na D ........... 3500–Na B ........... 3500–Na B–97.Ion Chromatography .......................... ............................... ............................... ............................... ................................. D 6919–03.

64. Specific conductance, micromhos/cm at 

25°C.

Wheatstone bridge ............................. 120.1 1 (Rev. 

1982).

2510 B .................. 2510 B .................. 2510 B–97 .............. D1125–95 (99) (A) 973.40 3, I–2781–

85 2

65. Sulfate (as SO4), mg/L ............................. Automated colorimetric ...................... 375.2, Rev. 2.0 

(1993).

Gravimetric ......................................... ............................... 4500–SO4 2–C or D 4500–SO4 2–C or D ................................. ............................... 925.54 3Turbidimetric ...................................... ............................... ............................... ............................... ................................. D516–90, 02 ......... 426C 30 Ion Chromatography .......................... 300.0, Rev 2.1 

(1993) and 300.1, Rev 1.0 (1997).

4110 B .................. 4110 B .................. 4110 B–00 .............. D4327–97, 03 ....... 993.30 3

CIE/UV ............................................... ............................... ............................... ............................... ................................. ............................... D6508, Rev. 2 54

66. Sulfide (as S), mg/L ................................. Titrimetric (iodine), or ......................... ............................... 4500–S2–F (19th) 

4500–S2–E (18th).

4500–S2–F ........... 4500–S2–F–00 ........ ............................... I–3840–85 2

Colorimetric (methylene blue) ............ ............................... 4500–S2–D ........... 4500–S2–D ........... 4500–S2–D–00.Ion Selective Electrode ...................... ............................... 4500–S2–G ........... 4500–S2–G ........... 4500–S2–G–00 ....... D4658–03.

67. Sulfite (as SO3), mg/L .............................. Titrimetric (iodine-iodate) ................... ............................... 4500–SO3 2–B ....... 4500–SO3 2–B ....... 4500–SO3 2–B–00.68. Surfactants, mg/L ..................................... Colorimetric (methylene blue) ............ ............................... 5540 C .................. 5540 C .................. 5540 C–00 .............. D2330–88, 02.69. Temperature, °C ....................................... Thermometric ..................................... ............................... 2550 B .................. 2550 B .................. 2550 B–00 .............. ............................... See footnote 3270. Thallium

—Total, 4 mg/L ............................ Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99.AA furnace ......................................... 279.2 1 (Issued 

1978).

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

(1994).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99.

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

71. Tin

—Total,4 mg/L ..................................... Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 B .................. ............................... 3111 B–99 .............. ............................... I–3850–78 8AA furnace, or .................................... ............................... 3113 B .................. ............................... 3113 B–99.STGFAA ............................................. 200.9, Rev. 2.2 

(1994).


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TABLE IB.

—

LIST OF

APPROVED INORGANIC

TEST

PROCEDURES

—Continued 

Parameter Methodology 58

Reference (method number or page) 

EPA35, 52 Standard methods (18th, 19th) Standard methods (20th) Standard methods online ASTM USGS/AOAC/other 

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

(1994).

72. Titanium

—Total,4 mg/L ............................. Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 D .................. ............................... 3111 D–99.AA furnace ......................................... 283.2 1 (Issued 

1978).

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

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

(1993).

2130 B .................. 2130 B .................. 2130 B–01 .............. D1889–94, 00 ....... I–3860–85 2

74. Vanadium

—Total,4 mg/L .......................... Digestion 4 followed by: 

AA direct aspiration ............................ ............................... 3111 D .................. ............................... 3111 D–99.AA furnace ......................................... ............................... ............................... ............................... ................................. D3373–93, 03.ICP/AES ............................................. 200.7, Rev. 4.4 

(1994).

3120 B .................. 3120 B .................. 3120 B–99 .............. ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP, or .............................................. ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Gallic Acid) ................... ............................... 3500–V D ............. 3500–V B ............. 3500–V B–97.

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

AA direct aspiration 36 ........................ ............................... 3111 B or C .......... ............................... 3111 B or C–99 ...... D1691–95, 02 (A 

or B).

974.27 3, p. 37 9, I–

3900–85 2

AA furnace ......................................... 289.2 1 (Issued 

1978).

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

(1994).

3120 B .................. 3120 B .................. 3120 B–99 59 ........... ............................... I–4471–97 50

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

(1994).

............................... ............................... ................................. D5673–03 ............. 993.14 3

DCP,36 or ........................................... ............................... ............................... ............................... ................................. D4190–94, 99 ....... See footnote 34Colorimetric (Dithizone) or ................. ............................... 3500–Zn E.(Zincon) .............................................. ............................... 3500–Zn F ............ 3500–Zn B ............ 3500–Zn B–97 ........ ............................... See footnote 33

Table 1B Notes: 1 ‘‘Methods for Chemical Analysis of Water and Wastes,’’ Environmental Protection Agency, Environmental Monitoring Systems Laboratory–Cincinnati (EMSL–CI), EPA–600/4–79–020 (NTIS PB 84–128677), Revised 

March 1983 and 1979 where applicable. 2Fishman, M. J., et al. ‘‘Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,’’ U.S. Department of the Interior, Techniques of Water-Resource Investigations of the U.S. Geological Survey, 

Denver, CO, Revised 1989, unless otherwise stated. 3 ‘‘Official Methods of Analysis of the Association of Official Analytical Chemists,’’ Methods Manual, Sixteenth Edition, 4th Revision, 1998. 4For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material 

and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non–platform graphite furnace atomic absorption determinations a digestion using nitric acid (as 

specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of ‘‘Methods for the Determination of Metals in Environmental Samples’’ EPA/600R–94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non–EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write–up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP–AES), the direct current plasma (DCP) technique or the EPA spectrochemical techniques (platform furnace AA, ICP–AES, and ICP–MS) use EPA Method 200.2 or an approved alternate procedure (e.g., CEM microwave digestion, which may be used with certain analytes 

as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as ‘‘total’’ metals. 5 Copper sulfate may be used in place of mercuric sulfate. 

6 Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to resolve any controversies. 7Ammonia, Automated Electrode Method, Industrial Method Number 379–75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 

10523. 8The approved method is that cited in ‘‘Methods for Determination of Inorganic Substances in Water and Fluvial Sediments’’, USGS TWRI, Book 5, Chapter A1 (1979). 9American National Standard on Photographic Processing Effluents, April 2, 1975. Available from ANSI, 25 West 43rd st., New York, NY 10036. 

10 ‘‘Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,’’ Supplement to the Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater 

(1981). 

11The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable. 12 Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ‘‘total BOD.’’ The addition of the nitrification inhibitor is not a procedural option, 

but must be included to report the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger’s permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor. 

13OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840. 14 Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 


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15The back titration method will be used to resolve controversy. 16Orion Research Instruction Manual, Residual Chlorine Electrode Model 97–70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138. The calibration graph for the Orion residual chlorine 

method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively. 

17The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976. 18 National Council of the Paper Industry for Air and Stream Improvement, Inc., Technical Bulletin 253, December 1971. 19 Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 20When using a method with block digestion, this treatment is not required. 21 Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378–75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran & Luebbe Analyzing Technologies, Inc., Elmsford, NY 

10523. 

22 Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 23 Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2–113 and 2–117, Hach Chemical Company, Loveland, CO 80537. 24Wershaw, R. L.,et al., ‘‘Methods for Analysis of Organic Substances in Water,’’ Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised 1987) p. 14. 25 Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537. 26 Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH. 27The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted at a pH of 10.0±0.2. The approved methods are given on pp 

576–81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 510C for the manual spectrometric procedure. 

28 R.F. Addison and R. G. Ackman, ‘‘Direct Determination of Elemental Phosphorus by Gas–Liquid Chromatography,’’ Journal of Chromatography, Vol. 47, No.3, pp. 421–426, 1970. 29Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of 

sample should be diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory. 

30The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition. 31For samples known or suspected to contain high levels of silver (e.g., in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2 to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the 

digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with NH4OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water. 

32Stevens, H.H., Ficke, J. F., and Smoot, G. F., ‘‘Water Temperature

—Influential Factors, Field Measurement and Data Presentation,’’ Techniques of Water-Resources Investigations of the U.S. Geological Survey, 

Book 1, Chapter D1, 1975. 

33Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2–231 and 2–333, Hach Chemical Company, Loveland, CO 80537. 34 ‘‘Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,’’ 1986

—Revised 1991, Thermo Jarrell Ash Corporation, 27 Forge 

Parkway, Franklin, MA 02038 

35Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC method for arsenic are provided in Appendix D of this part titled, 

‘‘Precision and Recovery Statements for Methods for Measuring Metals.’’

36 Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. ‘‘Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals’’, CEM Corporation, 

P.O. Box 200, Matthews, NC 28106–0200, April 16, 1992. Available from the CEM Corporation. 

37When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. 38Only use n-hexane extraction solvent when determining Oil and Grease parameters

—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Method 1664A). Use of other extraction 

solvents (e.g., those in the 18th and 19th editions) is prohibited. 

39 Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842. 40 Nitrogen, Total Kjeldahl, Method PAI–DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842. 41 Nitrogen, Total Kjeldahl, Method PAI–DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, OI Analytical/ALPKEM, P.O. Box 9010, College Station, TX 77842. 42 Method 1664, Revision A ‘‘n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry’’ EPA–821–

R–98–002, February 1999. Available at NTIS, PB–121949, U.S. Department of Commerce, 5285 Port Royal, Springfield, VA 22161. 

43 USEPA. 2001. Method 1631, Revision E, ‘‘Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry’’ September 2002, Office of Water, U.S. Environmental Protection 

Agency (EPA–821–R–02–024). The application of clean techniques described in EPA’s draft Method 1669: Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels (EPA–821–R–96–011) are 

recommended to preclude contamination at low-level, trace metal determinations. 

44Available Cyanide, Method OIA–1677, ‘‘Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,’’ ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842–9010. 45 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Ammonia Plus Organic Nitrogen by a Kjeldahl Digestion Method,’’ Open File Report (OFR) 00–170. 

46 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry,’’ Open File Report (OFR) 

93–449. 

47 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry,’’ Open File Report (OFR) 97–

198. 

48 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis’’ Open File Report (OFR) 92–146. 

49 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry’’

Open File Report (OFR) 98–639. 

50 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and 

Inductively Coupled Plasma-Mass Spectrometry,’’ Open File Report (OFR) 98-165. 

51 ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory

—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment,’’ Open File Report (OFR) 93–125. 

52All EPA methods, excluding EPA Method 300.1, are published in ‘‘Methods for the Determination of Metals in Environmental Samples,’’ Supplement I, National Exposure Risk Laboratory-Cincinnati (NERL–CI), 

EPA/600/R–94/111, May 1994; and ‘‘Methods for the Determination of Inorganic Substances in Environmental Samples,’’ NERL–CI, EPA/600/R–93/100, August, 1993. EPA Method 300.1 is available from http:// 

www.epa.gov/safewater/methods/pdfs/met300.pdf. 

53Styrene divinyl benzene beads (e.g. AMCO–AEPA–1 or equivalent) and stabilized formazin (e.g., Hach StablCalTM or equivalent) are acceptable substitutes for formazin. 54 Method D6508, Rev. 2, ‘‘Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,’’ available from Waters Corp, 34 Maple 

St., Milford, MA, 01757, Telephone: 508/482–2131, Fax: 508/482–3625. 

55Kelada-01, ‘‘Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate,’’ EPA 821–B–01–009, Revision 1.2, August 2001, National Technical Information Service (NTIS), 5285 

Port Royal Road, Springfield, VA 22161 [Order Number PB 2001–108275]. The toll free telephone number is: 800–553–6847. Note: A 450–W UV lamp may be used in this method instead of the 550–W lamp specified 

if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met. 

56QuikChem Method 10–204–00–1–X, ‘‘Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis’’ is available from Lachat 

Instruments 6645 W. Mill Road, Milwaukee, WI 53218, Telephone: 414–358–4200. 

57When using sulfide removal test procedures described in Method 335.4, reconstitute particulate that is filtered with the sample prior to distillation. 58 Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation ‘‘followed by’’ analysis with a method, approved digestion and/or distillation are required prior to analysis. 59 Method 245.7, Rev. 2.0, ‘‘Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry,’’ February 2005, EPA–821–R–05–001, available from the U.S. EPA Sample Control Center (operated by CSC), 6101 

Stevenson Avenue, Alexandria, VA 22304, Telephone: 703–461–2100, Fax: 703–461–8056. 


rwilkins on PROD1PC63 with RULES
11226 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 60The use of EDTA may decrease method sensitivity in some samples. Analysts may omit EDTA provided that all method specified quality control acceptance criteria are met. 61Samples analyzed for available cyanide using Methods OIA–1677 or D6888–04 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand ex- change reagents and sample analysis to no more than 30 minutes to preclude settling of materials in samples. 


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11227 

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

Parameter 1

EPA method number 2, 7 Other approved methods 

GC GC/MS HPLC Standard Methods 

[Edition(s)] 

Standard Methods 

Online ASTM Other 

1. Acenaphthene ............... 610 625, 1625B ..... 610 6440 B [18th, 19th, 

20th].

............................... D4657–92 (99) ..... See footnote 9, p. 

27 

2. Acenaphthylene ............ 610 625, 1625B ..... 610 6410 B, 6440 B, 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

3. Acrolein ......................... 603 624 4, 1624B.

4. Acrylonitrile .................... 603 624 4, 1624B.

5. Anthracene .................... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

6. Benzene ........................ 602 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B 

[18th,19th], 6200 

C [20th] and 

6220 B 

[18th,19th].

6200 B and C–97.

7. Benzidine ...................... ........................ 625 5, 1625B .. 605 ............................... ............................... ............................... See footnote 3, p.1 

8. Benzo(a)anthracene ...... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

9. Benzo(a)pyrene ............. 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

10. Benzo(b)fluoranthene .. 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

11. Benzo(g,h,i) perylene .. 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

12. Benzo(k) fluoranthene 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

13. Benzyl chloride ............ ........................ ........................ ........................ ............................... ............................... ............................... See footnote 3, p. 

130: See footnote 6, p. S102 

14. Benzyl butyl phthalate 606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

15. Bis(2-chloroethoxy) 

methane.

611 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

16. Bis(2-chloroethyl) ether 611 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

17. Bis(2-ethylhexyl) 

phthalate.

606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

18. Bromodichloro-methane.601 624, 1624B ..... ........................ 6200 C [20th] and 

6230 B [18th, 

19th], 6200 B 

[20th] and 6210 

B [18th, 19th].

6200 B and C–97.

19. Bromoform .................. 601 624, 1624B ..... ........................ 6200 C [20th] and 

6230 B [18th, 

19th], 6200 B 

[20th] and 6210 

B [18th, 19th].

6200 B and C–97.

20. Bromomethane ............ 601 624, 1624B ..... ........................ 6200 C [20th] and 

6230 B [18th, 

19th], 6200 B 

[20th] and 6210 

B [18th, 19th].

6200 B and C–97.

21. 4-Bromophenyl phenyl 

ether.

611 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

22. Carbon tetrachloride ... 601 624, 1624B ..... ........................ 6200 C [20th] and 

6230 B [18th, 

19th].

6200 C–97 ............ ............................... See footnote 3, p. 

130 

23. 4-Chloro-3-methyl phenol.604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

24. Chlorobenzene ............ 601, 602 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6220 

B [18th, 19th], 

6200 C [20th] 

and 6230 B 

[18th, 19th].

6200 B and C–97 ............................... See footnote 3, p. 

130 

25. Chloroethane ............... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

26. 2-Chloroethylvinyl 

ether.

601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.


rwilkins on PROD1PC63 with RULES
11228 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

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

Parameter 1

EPA method number 2, 7 Other approved methods 

GC GC/MS HPLC Standard Methods 

[Edition(s)] 

Standard Methods 

Online ASTM Other 

27. Chloroform .................. 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97 ............................... See footnote 3, p. 

130 

28. Chloromethane ............ 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th] 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

29. 2-Chloronaph-thalene 612 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

30. 2-Chlorophenol ............ 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B(00, 6420 

B–00.

............................... See footnote 9, p. 

27 

31. 4-Chlorophenyl phenyl 

ether.

611 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

32. Chrysene ..................... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

33. Dibenzo(a,h)anthracene.610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

34. Dibromochloro-methane.601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th] 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

35. 1,2-Dichloro-benzene .. 601, 602 624, 1625B ..... ........................ 6200 C [20th] and 

6220 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 C–97 ............ ............................... See footnote 9, p. 

27 

36. 1,3-Dichloro-benzene .. 601, 602 624, 1625B ..... ........................ 6200 C [20th] and 

6220 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 C–97 ............ ............................... See footnote 9, p. 

27 

37. 1,4-Dichloro-benzene .. 601, 602 624, 1625B ..... ........................ 6200 C [20th] and 

6220 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 C–97 ............ ............................... See footnote 9, p. 

27 

38. 3,3-Dichloro-benzidine ........................ 625, 1625B ..... 605 6410 B [18th, 19th, 

20th].

6410 B–00.

39. Dichlorodifluoro-methane.601 ........................ ........................ 6200 C [20th] and 

6230 B [18th, 

19th].

6200 C–97.

40. 1,1-Dichloroethane ...... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

41. 1,2-Dichloroethane ...... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

42. 1,1-Dichloroethene ...... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

43. trans-1,2-Dichloroethene.601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

44. 2,4-Dichlorophenol ...... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

45. 1,2-Dichloro-propane .. 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

46. cis-1,3-Dichloropropene.601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11229 

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

Parameter 1

EPA method number 2, 7 Other approved methods 

GC GC/MS HPLC Standard Methods 

[Edition(s)] 

Standard Methods 

Online ASTM Other 

47. trans-1,3-Dichloropropene.601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

48. Diethyl phthalate ......... 606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

49. 2,4-Dimethylphenol ..... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

50. Dimethyl phthalate ...... 606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

51. Di-n-butyl phthalate ..... 606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

52. Di-n-octyl phthalate ..... 606 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

53. 2,3-Dinitrophenol ......... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

...............................

54. 2,4-Dinitrotoluene ........ 609 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

55. 2,6-Dinitrotoluene ........ 609 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

56. Epichlorohydrin ........... ........................ ........................ ........................ ............................... ............................... ............................... See footnote 3, p. 

130; See footnote 6, p. S102 

57. Ethylbenzene .............. 602 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6220 

B [18th, 19th].

6200 B and C–97 ...............................

58. Fluoranthene ............... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

59. Fluorene ...................... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

60. 1,2,3,4,6,7,8- 

Heptachlorodibenzofuran.

........................ 1613B10.

61. 1,2,3,4,7,8,9- 

Heptachlorodibenzofuran.

1613B10.

62. 1,2,3,4,6,7,8- 

Heptachlorodibenzo-pdioxin.

........................ 1613B10.

63. Hexachlorobenzene .... 612 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

64. Hexachloro-butadiene 612 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

65. Hexachlorocyclopentadiene.612 625 5, 1625B .. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

66. 1,2,3,4,7,8- 

Hexachlorodibenzofuran.

........................ 1613B10.

67. 1,2,3,6,7,8- 

Hexachlorodibenzofuran.

........................ 1613B10.

68. 1,2,3,7,8,9- 

Hexachlorodibenzofuran.

........................ 1613B10.

69. 2,3,4,6,7,8- 

Hexachlorodibenzofuran.

........................ 1613B10.

70. 1,2,3,4,7,8- 

Hexachlorodibenzo-pdioxin.

........................ 1613B10.

71. 1,2,3,6,7,8- 

Hexachlorodibenzo-pdioxin.

........................ 1613B10.

72. 1,2,3,7,8,9- 

Hexachlorodibenzo-pdioxin 1613B10.

........................ 1613B10.

73. Hexachloroethane ....... 612 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

74. Ideno(1,2,3-cd) pyrene 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

75. Isophorone .................. 609 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

76. Methylene chloride ...... 601 624, 1624B ..... ........................ 6200 C [20th] and 

6230 B [18th, 

19th].

6200 C–97 ............ ............................... See footnote 3, p. 

130 

77. 2-Methyl-4,6- 

dinitrophenol.

604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

78. Naphthalene ................ 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 


rwilkins on PROD1PC63 with RULES
11230 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

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

Parameter 1

EPA method number 2, 7 Other approved methods 

GC GC/MS HPLC Standard Methods 

[Edition(s)] 

Standard Methods 

Online ASTM Other 

79. Nitrobenzene ............... 609 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

80. 2-Nitrophenol ............... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

81. 4-Nitrophenol ............... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

82. NNitrosodimethylamine.

607 6255, 1625B ... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

83. N-Nitrosodi-n-propylamine.607 6255, 1625B ... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

84. NNitrosodiphenylamine.607 6255, 1625B ... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 9, p. 

27 

85. 

Octachlorodibenzofuran.

........................ 1613B10*.

86. Octachlorodibenzo-pdioxin......................... 1613B10.

87. 2,2’-Oxybis(2- 

chloropropane) [also 

known as bis(2- 

chloroisopropyl) ether].

611 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00.

88. PCB–1016 ................... 608 625 ................. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 8

89. PCB–1221 ................... 608 625 ................. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 8

90. PCB–1232 ................... 608 625 ................. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 8

91. PCB–1242 ................... 608 625 ................. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 

8

92. PCB–1248 ................... 608 625.

93. PCB–1254 ................... 608 625 ................. ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 

8

94. PCB–1260 ................... 608 625 ................. ........................ 6410 B, 6630 B 

[18th, 19th, 20th].

6410 B–00 ............ ............................... See footnote 3, p. 

43; See footnote 

8 

95. 1,2,3,7,8-Pentachlorodibenzofuran ......................... 1613B10.

96. 2,3,4,7,8-Pentachlorodibenzofuran ......................... 1613B10.

97. 1,2,3,7,8,- 

Pentachlorodibenzo-pdioxin.

........................ 1613B10.

98. Pentachlorophenol ...... 604 625, 1625B ..... ........................ 6410 B, 6630 B 

[18th, 19th, 20th].

6410 B–00 ............ ............................... See footnote 3, p. 

140; See footnote 9, p. 27 

99. Phenanthrene .............. 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

100. Phenol ....................... 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

101. Pyrene ....................... 610 625, 1625B ..... 610 6410 B, 6440 B 

[18th, 19th, 20th].

6410 B–00 ............ D4657–92 (99) ..... See footnote 9, p. 

27 

102. 2,3,7,8-Tetrachlorodibenzofuran......................... 1613B10.

103. 2,3,7,8-Tetrachlorodibenzo-p-dioxin......................... 613, 625 5a, 

1613B10.

104. 1,1,2,2-Tetra-chloro 

ethane .

601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97 ............................... See footnote 3, p. 

130 

105. Tetrachloroethene ..... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97 ............................... See footnote 3, p. 

130 

106. Toluene ..................... 602 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6220 

B [18th, 19th].

6200 B and C–97.

107. 1,2,4-Trichloro-benzene.612 625, 1625B ..... ........................ 6410 B [18th, 19th, 

20th].

6410 B–00 ............ ............................... See footnote 3, p. 

130; See footnote 9, p. 27 


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11231 

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

Parameter 1

EPA method number 2, 7 Other approved methods 

GC GC/MS HPLC Standard Methods 

[Edition(s)] 

Standard Methods 

Online ASTM Other 

108. 1,1,1-Trichloro-ethane 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

109. 1,1,2-Trichloro-ethane 601 624, 1624B ..... 6200 B [20th] 

and 6210 B 

[18th, 19th], 

6200 C [20th] 

and 6230 B 

[18th, 19th] 

6200 B and C–97 ............................... See footnote 3, p. 

130.

110. Trichloroethene ......... 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

111. Trichlorofluoro-methane.601 624 ................. ........................ 6200 B [20th] and 

6210 B [18th, 

19th], 6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

112. 2,4,6-Trichlorophenol 604 625, 1625B ..... ........................ 6410 B, 6420 B 

[18th, 19th, 20th].

6410 B–00, 6420 

B–00.

............................... See footnote 9, p. 

27 

113. Vinyl chloride ............. 601 624, 1624B ..... ........................ 6200 B [20th] and 

6210 B [18th, 

19th], ≤6200 C 

[20th] and 6230 

B [18th, 19th].

6200 B and C–97.

1All parameters are expressed in micrograms per liter (μg/L) except for Method 1613B in which the parameters are expressed in picograms per liter (pg/L). 2The full text of Methods 601–613, 624, 625, 1624B, and 1625B, are given at Appendix A, ‘‘Test Procedures for Analysis of Organic Pollutants,’’ of this Part 136. 

The full text of Method 1613B is incorporated by reference into this Part 136 and is available from the National Technical Information Services as stock number 

PB95–104774. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ‘‘Definition and Procedure for the Determination of the Method Detection Limit,’’ of this Part 136. 3 ‘‘Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,’’ U.S. Environmental Protection Agency, 

September, 1978. 4 Method 624 may be extended to screen samples for Acrolein and Acrylonitrile. However, when they are known to be present, the preferred method for these two 

compounds is Method 603 or Method 1624B. 5 Method 625 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine. However, when they are 

known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds. 5a 625, screening only. 6 ‘‘Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,’’ Supplement to the Fifteenth Edition of Standard Methods for the Examination of Water and Wastewater (1981). 7Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601–603, 624, 625, 1624B, 

and 1625B (See Appendix A of this Part 136) in accordance with procedures each in Section 8.2 of each of these methods. Additionally, each laboratory, on an ongoing basis must spike and analyze 10% (5% for methods 624 and 625 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory 

data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for 

that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control 

requirements also apply to the Standard Methods, ASTM Methods, and other methods cited. 8 ‘‘Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk’’ 3M Corporation Revised 10/28/94. 9 USGS Method 0–3116–87 from ‘‘Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments,’’ U.S. Geological Survey, Open File Report 93–125. 10Analysts may use Fluid Management Systems, Inc. PowerPrep system in place of manual cleanup provided that the analysis meet the requirements of Method 

1613B (as specified in Section 9 of the method) and permitting authorities. 

TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1

Parameter Method EPA2, 7 Standard Methods 

18th, 19th, 20th Ed. 

Standard Methods 

Online ASTM Other 

1. Aldrin .............................. GC .................. 608 6630 B & C .......... .......................... D3086–90, ............

D5812-96 (2002) ..

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

27; See footnote 8

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

2. Ametryn .......................... GC .................. ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p S68 

3. Aminocarb ...................... TLC ................ ............................... ............................... ............................... See footnote 3, p. 94; See footnote 6, 

p. S16 

4. Atraton ............................ GC .................. ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68 

5. Atrazine .......................... GC .................. ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68; See footnote 9

6. Azinphos methyl ............. GC .................. ............................... ............................... ............................... See footnote 3, p. 25; See footnote 6, 

p. S51 

7. Barban ............................ TLC ................ ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

8. a–BHC ........................... GC .................. 608 6630 B & C .......... .......................... D3086–90, ............

D5812–96(02) ......

See footnote 3, p. 7; See footnote 8

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

9. b–BHC ............................ GC .................. 608 6630 C .................. .......................... D3086–90, ............

D5812–96(02) ......

See footnote 8

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


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11232 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued 

Parameter Method EPA2, 7 Standard Methods 

18th, 19th, 20th Ed. 

Standard Methods 

Online ASTM Other 

10. d–BHC .......................... GC .................. 608 6630 C .................. .......................... D3086–90, ............

D5812–96(02) ......

See footnote 8

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

11. g-BHC (Lindane) ........... GC .................. 608 6630 B & C .......... .......................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

.

12. Captan .......................... GC .................. .................... 6630 B .................. ............................... D3086–90, ............

D5812–96(02) ......

See footnote 3, p. 7 

13. Carbaryl ........................ TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 94, See footnote 6, 

p. S60 

14. Carbo-phenothion ......... GC .................. .................... ............................... ............................... ............................... See footnote 4, p. 27; See footnote 6, 

p. S73 

15. Chlordane ..................... GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

16. Chloro-propham ........... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64. 

17. 2,4-D ............................. GC .................. .................... 6640 B .................. ............................... ............................... See footnote 3, p. 115; See footnote 4, 

p. 40 

18. 4,4′-DDD ...................... GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

19. 4,4′-DDE ....................... GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

20. 4,4′-DDT ....................... GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

21. Demeton-O ................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 25; See footnote 6, 

p. S51 

22. Demeton-S ................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 25; See footnote 6, 

p. S51 

23. Diazinon ....................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 25; See footnote 4, 

p. 27; See footnote 6, p. S51 

24. Dicamba ....................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 115 

25. Dichlofen-thion ............. GC .................. .................... ............................... ............................... ............................... See footnote 4, p. 27; See footnote 6, 

p. S73 

26. Dichloran ...................... GC .................. .................... 6630 B & C .......... ............................... ............................... See footnote 3, p. 7 

27. Dicofol .......................... GC .................. .................... ............................... ............................... D3086–90, ............

D5812–96(02).

28. Dieldrin ......................... GC .................. 608 6630 B & C .......... ............................... ............................... See footnote 3, p. 7; See footnote 4, p. 

27; See footnote 8

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

29. Dioxathion .................... GC .................. .................... ............................... ............................... ............................... See footnote 4, p. 27; See footnote 6, 

p. S73 

30. Disulfoton ..................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 25; See footnote 6, 

p. S51 

31. Diuron ........................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

32. Endosulfan I ................. GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

33. Endosulfan II ................ GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

See footnote 3, p. 7; See footnote 8

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

34. Endosulfan Sulfate ....... GC .................. 608 6630 C .................. ............................... ............................... See footnote 8

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

35. Endrin ........................... GC .................. 608 6630 B & C .......... ............................... D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

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

36. Endrin aldehyde ........... GC ..................

GC/MS ...........

608 

625 

............................... ............................... ............................... See footnote 8

37. Ethion ........................... GC .................. .................... ............................... ............................... ............................... See footnote 4, p. 27; See footnote 6, 

p. S73 

38. Fenuron ........................ TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

39. Fenuron-TCA ................ TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

40. Heptachlor .................... GC ..................

GC/MS ...........

608 

625 

6630 B & C ..........

6410 B ..................

...............................

6410 B–00.

D3086–90, ............

D5812–96(02) ......

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

27; See footnote 8

41. Heptachlor epoxide ...... GC ..................

GC/MS ...........

608 

625 

6630 B & C ..........

6410 B ..................

...............................

6410 B–00.

D3086–90, ............

D5812– 96(02) .....

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

27; See footnote 6, p. S73; See 

footnote 8

42. Isodrin ........................... GC .................. .................... ............................... ............................... ............................... See footnote 4, p. 27; See footnote 6, 

p. S73 

43. Linuron ......................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

44. Malathion ...................... GC .................. .................... 6630 C .................. ............................... ............................... See footnote 3, p. 25; See footnote 4, 

p. 27; See footnote 6, p. S51 


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11233 

TABLE ID.—LIST OF APPROVED TEST PROCEDURES FOR PESTICIDES 1—Continued 

Parameter Method EPA2, 7 Standard Methods 

18th, 19th, 20th Ed. 

Standard Methods 

Online ASTM Other 

45. Methiocarb .................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 94; See footnote 6, 

p. S60 

46. Methoxy-chlor ............... GC .................. .................... 6630 B & C .......... ............................... D3086–90, 

D5812–96(02).

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

27; See footnote 8

47. Mexacar-bate ............... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 94; See footnote 6, 

p.S60 

48. Mirex ............................. GC .................. .................... 6630 B & C .......... ............................... ............................... See footnote 3, p. 7; See footnote 4, p. 

27 

49. Monuron ....................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

50. Monuron-TCA ............... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

51. Nuburon ........................ TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

52. Parathion methyl .......... GC .................. .................... 6630 C .................. ............................... ............................... See footnote 3, p. 25; See footnote 4, 

p. 27 

53. Parathion ethyl ............. GC .................. .................... 6630 C .................. ............................... ............................... See footnote 3, p. 25; See footnote 4, 

p. 27 

54. PCNB ........................... GC .................. .................... 6630 B & C .......... ............................... ............................... See footnote 3, p. 7 

55. Perthane ....................... GC .................. .................... ............................... ............................... D3086–90, 

D5812–96(02).

See footnote 4, p. 27 

56. Prometon ...................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68; See footnote 9

57. Prometryn ..................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68; See footnote 9

58. Propazine ..................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68; See footnote 9

59. Propham ....................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

60. Propoxur ....................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 94; See footnote 6, 

p. S60 

61. Secbumeton ................. TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68 

62. Siduron ......................... TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

63. Simazine ....................... GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68; See footnote 9

64. Strobane ....................... GC .................. .................... 6630 B & C .......... ............................... ............................... See footnote 3, p. 7 

65. Swep ............................ TLC ................ .................... ............................... ............................... ............................... See footnote 3, p. 104; See footnote 6, 

p. S64 

66. 2,4,5–T ......................... GC .................. .................... 6640 B .................. ............................... ............................... See footnote 3, p. 115; See footnote 4, 

p. 40 

67. 2,4,5–TP (Silvex) .......... GC .................. .................... 6640 B .................. ............................... ............................... See footnote 3, p. 115; See footnote 4, 

p. 40 

68. Terbuthylazine .............. GC .................. .................... ............................... ............................... ............................... See footnote 3, p. 83; See footnote 6, 

p. S68 

69. Toxaphene ................... GC .................. 608 6630 B & C .......... ............................... D3086–90, 

D5812–96(02).

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

27; See footnote 8

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

70. Trifluralin ....................... GC .................. .................... 6630 B .................. ............................... ............................... See footnote 3, p. 7; See footnote 9

1Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where entries are listed by chemical name. 2The full text of Methods 608 and 625 are given at Appendix A, ‘‘Test Procedures for Analysis of Organic Pollutants,’’ of this Part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ‘‘Definition and Procedure for the Determination of the Method Detection Limit,’’ of this Part 136. 3 ‘‘Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,’’ U.S. Environmental Protection Agency, September 1978. This 

EPA publication includes thin-layer chromatography (TLC) methods. 4‘‘Methods for Analysis of Organic Substances in Water and Fluvial Sediments,’’ Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3 (1987). 5The method may be extended to include a-BHC, g-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608 is the preferred method. 6 ‘‘Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.’’ Supplement to the Fifteenth Edition of Standard Methods for the Examination of 

Water and Wastewater (1981). 7Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625 (See Appendix A of this Part 136) in 

accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 10% of all samples analyzed with 

Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of 

any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited. 8 ‘‘Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk’’, 3M Corporation, Revised 10/28/94. 9 USGS Method 0–3106–93 from ‘‘Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Triazine and Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors’’ U.S. Geological Survey Open File Report 94–37. 

TABLE IE.—LIST OF APPROVED RADIOLOGIC TEST TEST PROCEDURES

Parameter and units Method 

Reference (method number or page) 

EPA1

Standard Methods 18th, 19th, 

20th Ed. 

Standard Methods Online ASTM USGS2

1. Alpha-Total, pCi per 

liter.

Proportional or scintillation counter.900.0 ........... 7110 B ................ 7110 B–00 .......... D1943–90, 96 .... pp. 75 and 78 3

2. Alpha-Counting 

error, pCi per liter.

Proportional or scintillation counter.Appendix B .. 7110 B ................ 7110 B–00 .......... D1943–90, 96 .... p. 79 

3. Beta-Total, pCi per 

liter.

Proportional counter ... 900.0 ........... 7110 B ................ 7110 B–00 .......... D1890–90, 96 .... pp. 75 and 78 3


rwilkins on PROD1PC63 with RULES
11234 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE IE.—LIST OF APPROVED RADIOLOGIC TEST TEST PROCEDURES—Continued 

Parameter and units Method 

Reference (method number or page) 

EPA1

Standard Methods 18th, 19th, 

20th Ed. 

Standard Methods Online ASTM USGS2

4. Beta-Counting error, 

pCi.

Proportional counter ... Appendix B .. 7110 B ................ 7110 B–00 .......... D1890–90, 96 ..... p. 79 

5. (a) Radium Total 

pCi per liter.

(b) Ra, pCi per liter ....

Proportional counter ... 903.0 ........... 7500-Ra B .......... 7500-Ra B–01 .... D2460–90, 97 .....

Scintillation counter .... 903.1 ........... 7500-Ra C .......... 7500-Ra C–01 .... D3454–91, 97 ..... p. 81 

1Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA–600/4–80–032 (1980), U.S. Environmental Protection Agency, August 1980. 2Fishman, M. J. and Brown, Eugene, ‘‘Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters,’’ U.S. Geological Survey, 

Open-File Report 76–177 (1976). 3The method found on p. 75 measures only the dissolved portion while the method on p. 78 measures only the suspended portion. Therefore, 

the two results must be added to obtain the ‘‘total.’’

* * * * * 

TABLE IG.—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS

EPA Survey 

Code Pesticide name CAS No. EPA Analytical Method No.(s) 

8 .................. Triadimefon ........................................................................................................................... 43121–43–3 507/633/525.1/1656 

12 ................ Dichlorvos .............................................................................................................................. 62–73–7 1657/507/622/525.1 

16 ................ 2,4–D; 2,4–D Salts and Esters [2,4–Dichloro-phenoxyacetic acid] ...................................... 94–75–7 1658/515.1/615/515.2/555 

17 ................ 2,4–DB; 2,4–DB Salts and Esters [2,4–Dichlorophenoxybutyric acid] ................................. 94–82–6 1658/515.1/615/515.2/555 

22 ................ Mevinphos ............................................................................................................................. 7786–34–7 1657/507/622/525.1 

25 ................ Cyanazine ............................................................................................................................. 21725–46–2 629/507 

26 ................ Propachlor ............................................................................................................................. 1918–16–7 1656/508/608.1/525.1 

27 ................ MCPA; MCPA Salts and Esters [2–Methyl-4-chlorophenoxyacetic acid] ............................. 94–74–6 1658/615/555 

30 ................ Dichlorprop; Dichlorprop Salts and Esters [2–(2,4–Dichlorophenoxy) propionic acid] ......... 120–36–5 1658/515.1/615/515.2/555 

31 ................ MCPP; MCPP Salts and Esters [2–(2–Methyl-4-chlorophenoxy) propionic acid] ................ 93–65–2 1658/615/555 

35 ................ TCMTB [2–(Thiocyanomethylthio) benzo-thiazole] ............................................................... 21564–17–0 637 

39 ................ Pronamide ............................................................................................................................. 23950–58–5 525.1/507/633.1 

41 ................ Propanil ................................................................................................................................. 709–98–8 632.1/1656 

45 ................ Metribuzin .............................................................................................................................. 21087–64–9 507/633/525.1/1656 

52 ................ Acephate ............................................................................................................................... 30560–19–1 1656/1657 

53 ................ Acifluorfen ............................................................................................................................. 50594–66–6 515.1/515.2/555 

54 ................ Alachlor ................................................................................................................................. 15972–60–8 505/507/645/525.1/1656 

55 ................ Aldicarb ................................................................................................................................. 116–06–3 531.1 

58 ................ Ametryn ................................................................................................................................. 834–12–8 507/619/525.1 

60 ................ Atrazine ................................................................................................................................. 1912–24–9 505/507/619/525.1/1656 

62 ................ Benomyl ................................................................................................................................ 17804–35–2 631 

68 ................ Bromacil; Bromacil Salts and Esters .................................................................................... 314–40–9 507/633/525.1/1656 

69 ................ Bromoxynil ............................................................................................................................. 1689–84–5 1625/1661 

69 ................ Bromoxynil octanoate ............................................................................................................ 1689–99–2 1656 

70 ................ Butachlor ............................................................................................................................... 23184–66–9 507/645/525.1/1656 

73 ................ Captafol ................................................................................................................................. 2425–06–1 1656 

75 ................ Carbaryl [Sevin] ..................................................................................................................... 63–25–2 531.1/632/553 

76 ................ Carbofuran ............................................................................................................................ 1563–66–2 531.1/632 

80 ................ Chloroneb .............................................................................................................................. 2675–77–6 1656/508/608.1/525.1 

82 ................ Chlorothalonil ........................................................................................................................ 1897–45–6 508/608.2/525.1/1656 

84 ................ Stirofos .................................................................................................................................. 961–11–5 1657/507/622/525.1 

86 ................ Chlorpyrifos ........................................................................................................................... 2921–88–2 1657/508/622 

90 ................ Fenvalerate ........................................................................................................................... 51630–58–1 1660 

103 .............. Diazinon ................................................................................................................................ 333–41–5 1657/507/614/622/525.1 

107 .............. Parathion methyl ................................................................................................................... 298–00–0 1657/614/622 

110 .............. DCPA [Dimethyl 2,3,5,6-tetrachloro-terephthalate] ............................................................... 1861–32–1 508/608.2/525.1/515.1/515.2/1656 

112 .............. Dinoseb ................................................................................................................................. 88–85–7 1658/515.1/615/515.2/555 

113 .............. Dioxathion ............................................................................................................................. 78–34–2 1657/614.1 

118 .............. Nabonate [Disodium cyanodithio-imidocarbonate] ............................................................... 138–93–2 630.1 

119 .............. Diuron .................................................................................................................................... 330–54–1 632/553 

123 .............. Endothall ............................................................................................................................... 145–73–3 548/548.1 

124 .............. Endrin .................................................................................................................................... 72–20–8 1656/505/508/608/617/525.1 

125 .............. Ethalfluralin ............................................................................................................................ 55283–68–6 1656/627 See footnote 1 

126 .............. Ethion .................................................................................................................................... 563–12–2 1657/614/614.1 

127 .............. Ethoprop ................................................................................................................................ 13194–48–4 1657/507/622/525.1 

132 .............. Fenarimol .............................................................................................................................. 60168–88–9 507/633.1/525.1/1656 

133 .............. Fenthion ................................................................................................................................ 55–38–9 1657/622 

138 .............. Glyphosate [N(Phosphonomethyl) glycine] ........................................................................... 1071–83–6 547 

140 .............. Heptachlor ............................................................................................................................. 76–44–8 1656/505/508/608/617/525.1 

144 .............. Isopropalin ............................................................................................................................. 33820–53–0 1656/627 

148 .............. Linuron .................................................................................................................................. 330–55–2 553/632 

150 .............. Malathion ............................................................................................................................... 121–75–5 1657/614 

154 .............. Methamidophos ..................................................................................................................... 10265–92–6 1657 

156 .............. Methomyl ............................................................................................................................... 16752–77–5 531.1/632 


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Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11235 

TABLE IG.—TEST METHODS FOR PESTICIDE ACTIVE INGREDIENTS—Continued 

EPA Survey 

Code Pesticide name CAS No. EPA Analytical Method No.(s) 

158 .............. Methoxychlor ......................................................................................................................... 72–43–5 1656/505/508/608.2/617/525.1 

172 .............. Nabam ................................................................................................................................... 142–59–6 630/630.1 

173 .............. Naled ..................................................................................................................................... 300–76–5 1657/622 

175 .............. Norflurazon ............................................................................................................................ 27314–13–2 507/645/525.1/1656 

178 .............. Benfluralin ............................................................................................................................. 1861–40–1 11656/1627 

182 .............. Fensulfothion ......................................................................................................................... 115–90–2 1657/622 

183 .............. Disulfoton .............................................................................................................................. 298–04–4 1657/507/614/622/525.1 

185 .............. Phosmet ................................................................................................................................ 732–11–6 1657/622.1 

186 .............. Azinphos Methyl .................................................................................................................... 86–50–0 1657/614/622 

192 .............. Organo-tin pesticides ............................................................................................................ 12379–54–3 Ind-01/200.7/200.9 

197 .............. Bolstar ................................................................................................................................... 35400–43–2 1657/622 

203 .............. Parathion ............................................................................................................................... 56–38–2 1657/614 

204 .............. Pendimethalin ........................................................................................................................ 40487–42–1 1656 

205 .............. Pentachloronitrobenzene ...................................................................................................... 82–68–8 1656/608.1/617 

206 .............. Pentachlorophenol ................................................................................................................ 87–86–5 625/1625/515.2/555/515.1/ 525.1 

208 .............. Permethrin ............................................................................................................................. 52645–53–1 608.2/508/525.1/1656/1660 

212 .............. Phorate .................................................................................................................................. 298–02–2 1657/622 

218 .............. Busan 85 [Potassium dimethyldithiocarbamate] ................................................................... 128–03–0 630/630.1 

219 .............. Busan 40 [Potassium N-hydroxymethyl-N-methyldithiocarbamate] ...................................... 51026–28–9 630/630.1 

220 .............. KN Methyl [Potassium N-methyl-dithiocarbamate] ............................................................... 137–41–7 630/630.1 

223 .............. Prometon ............................................................................................................................... 1610–18–0 507/619/525.1 

224 .............. Prometryn .............................................................................................................................. 7287–19–6 507/619/525.1 

226 .............. Propazine .............................................................................................................................. 139–40–2 507/619/525.1/1656 

230 .............. Pyrethrin I .............................................................................................................................. 121–21–1 1660 

232 .............. Pyrethrin II ............................................................................................................................. 121–29–9 1660 

236 .............. DEF [S,S,S–Tributyl phosphorotrithioate] ............................................................................. 78–48–8 1657 

239 .............. Simazine ................................................................................................................................ 122–34–9 505/507/619/525.1/1656 

241 .............. Carbam-S [Sodium dimethyldithiocarbanate] ....................................................................... 128–04–1 630/630.1 

243 .............. Vapam [Sodium methyldithiocarbamate] .............................................................................. 137–42–8 630/630.1 

252 .............. Tebuthiuron ........................................................................................................................... 34014–18–1 507/525.1 

254 .............. Terbacil .................................................................................................................................. 5902–51–2 507/633/525.1/1656 

255 .............. Terbufos ................................................................................................................................ 13071–79–9 1657/507/614.1/525.1 

256 .............. Terbuthylazine ....................................................................................................................... 5915–41–3 619/1656 

257 .............. Terbutryn ............................................................................................................................... 886–50–0 507/619/525.1 

259 .............. Dazomet ................................................................................................................................ 533–74–4 630/630.1/1659 

262 .............. Toxaphene ............................................................................................................................ 8001–35–2 1656/505/508/608/617/525.1 

263 .............. Merphos [Tributyl phosphorotrithioate] ................................................................................. 150–50–5 1657/507/525.1/622 

264 .............. Trifluralin ................................................................................................................................ 1582–09–8 1656/508/617/627/525.1 

268 .............. Ziram [Zinc dimethyldithiocarbamate] ................................................................................... 137–30–4 630/630.1 

1 Monitor and report as total Trifluralin. 

(b) * * * 

References, Sources, Costs, and Table 

Citations 

* * * * * 

(6) American Public Health 

Association. 1992, 1995, and 1998. 

Standard Methods for the Examination 

of Water and Wastewater. 18th, 19th, 

and 20th Edition (respectively). 

Available from: American Public Health 

Association, 1015 15th Street, NW., 

Washington, DC 20005. Standard 

Methods Online are available through 

the Standard Methods Web site (http:// 

www.standardmethods.org). Tables IA, 

IB, IC, ID, IE. 

* * * * * 

(10) ASTM International. Annual 

Book of ASTM Standards, Water, and 

Environmental Technology, Section 11, 

Volumes 11.01 and 11.02, 1994, 1996, 

1999, Volume 11.02, 2000, and 

individual standards published after 

2000. Available from: ASTM 

International, 100 Barr Harbor Drive, 

P.O. Box C700, West Conshohocken, PA 

19428–2959, or http://www.astm.org. 

Tables IA, IB, IC, ID, and IE. 

* * * * * 

(17) AOAC-International. Official 

Methods of Analysis of AOACInternational, 16th Edition, (1995). 

Available from: AOAC-International, 

481 North Frederick Avenue, Suite 500, 

Gaithersburg, MD 20877. Table IB, See 

footnote 3. 

* * * * * 

(63) Waters Corporation. Method 

D6508, Rev. 2, ‘‘Test Method for 

Determination of Dissolved Inorganic 

Anions in Aqueous Matrices Using 

Capillary Ion Electrophoresis and 

Chromate Electrolyte,’’ available from 

Waters Corp, 34 Maple Street, Milford, 

MA 01757, Telephone: 508/482–2131, 

Fax: 508/482–3625, Table IB, See 

footnote 54. 

(64) Kelada-01, ‘‘Kelada Automated 

Test Methods for Total Cyanide, Acid 

Dissociable Cyanide, and Thiocyanate,’’

EPA 821–B–01–009 Revision 1.2, 

August 2001 is available from National 

Technical Information Service (NTIS), 

5285 Port Royal Road, Springfield, VA 

22161 [Order Number PB 2001–108275]. 

Telephone: 800–553–6847. Table IB, See 

footnote 55. 

(65) QuikChem Method 10–204–00–

1–X, ‘‘Digestion and Distillation of Total 

Cyanide in Drinking and Wastewaters 

using MICRO DIST and Determination 

of Cyanide by Flow Injection Analysis’’

Revision 2.2, March 2005 is available 

from Lachat Instruments 6645 W. Mill 

Road, Milwaukee, WI 53218, Telephone: 

414–358–4200. Table IB, See footnote 

56. 

(66) ‘‘Methods for the Determination 

of Metals in Environmental Samples,’’

Supplement I, National Exposure Risk 

Laboratory-Cincinnati (NERL–CI), EPA/ 

600/R–94/111, May 1994; and ‘‘Methods 

for the Determination of Inorganic 

Substances in Environmental Samples,’’

NERL–CI, EPA/600/R–93/100, August, 

1993 are available from National 

Technical Information Service (NTIS), 

5285 Port Royal Road, Springfield, VA 

22161. Telephone: 800–553–6847. Table 

IB. 

(67) ‘‘Determination of Inorganic Ions 

in Drinking Water by Ion 

Chromatography,’’ Rev. 1.0, 1997 is 

available from from http://www.epa.gov/ 

safetwater/methods/met300.pdf. Table 

IB. 

(68) Table IG Methods are available in 

‘‘Methods For The Determination of 

Nonconventional Pesticides In 


rwilkins on PROD1PC63 with RULES
11236 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

Municipal and Industrial Wastewater, 

Volume I,’’ EPA 821–R–93–010A, 

August 1993 Revision I, and ‘‘Methods 

For The Determination of 

Nonconventional Pesticides In 

Municipal and Industrial Wastewater, 

Volume II,’’ EPA 821–R–93–010B 

(August 1993) are available from 

National Technical Information Service 

(NTIS), 5285 Port Royal Road, 

Springfield, VA 22161. Telephone: 800–

553–6847. 

(69) Method 245.7, Rev. 2.0, ‘‘Mercury 

in Water by Cold Vapor Atomic 

Fluorescence Spectrometry,’’ February 

2005, EPA–821–R–05–001, available 

from the U.S. EPA Sample Control 

Center (operated by CSC), 6101 

Stevenson Avenue, Alexandria, VA 

22304, Telephone: 703–461–8056. Table 

IB, See footnote 59. 

(c) Under certain circumstances, the 

Regional Administrator or the Director 

in the Region or State where the 

discharge will occur may determine for 

a particular discharge that additional 

parameters or pollutants must be 

reported. Under such circumstances, 

additional test procedures for analysis 

of pollutants may be specified by the 

Regional Administrator, or the Director 

upon recommendation of the Alternate 

Test Procedure Program Coordinator, 

Washington, DC. 

(d) Under certain circumstances, the 

Administrator may approve additional 

alternate test procedures for nationwide 

use, upon recommendation by the 

Alternate Test Procedure Program 

Coordinator, Washington, DC. 

(e) Sample preservation procedures, 

container materials, and maximum 

allowable holding times for parameters 

are cited in Tables IA, IB, IC, ID, IE, IF, 

and IG are prescribed in Table II. 

Information in the table takes 

precedence over information in specific 

methods or elsewhere. Any person may 

apply for a variance from the prescribed 

preservation techniques, container 

materials, and maximum holding times 

applicable to samples taken from a 

specific discharge. Applications for 

variances may be made by letters to the 

Regional Administrator in the Region in 

which the discharge will occur. 

Sufficient data should be provided to 

assure such variance does not adversely 

affect the integrity of the sample. Such 

data will be forwarded by the Regional 

Administrator, to the Alternate Test 

Procedure Program Coordinator, 

Washington, DC, for technical review 

and recommendations for action on the 

variance application. Upon receipt of 

the recommendations from the Alternate 

Test Procedure Program Coordinator, 

the Regional Administrator may grant a 

variance applicable to the specific 

discharge to the applicant. A decision to 

approve or deny a variance will be made 

within 90 days of receipt of the 

application by the Regional 

Administrator. 

TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES

Parameter number/name Container 1 Preservation 2,3 Maximum holding time 4

Table lA—Bacterial Tests: 

1–5. Coliform, total, fecal, and E. coli .......................................................................... PA, G ......................... Cool, <10 °C, 

0.0008% 

Na2S2O3 5.

6 hours 

6. Fecal streptococci ..................................................................................................... PA, G ......................... Cool, <10 °C, 

0.0008% 

Na2S2O3 5.

6 hours 

7. Enterococci ............................................................................................................... PA, G ......................... Cool, <10 °C, 

0.0008% 

Na2S2O3 5.

6 hours 

Table lA—Protozoan Tests: 

8. Cryptosporidium ........................................................................................................ LDPE; field filtration ... 0–8 °C ............. 96 hours 21

9. Giardia ...................................................................................................................... LDPE; field filtration ... 0–8 °C ............. 96 hours 21

Table lA—Aquatic Toxicity Tests: 

10–13. Toxicity, acute and chronic ............................................................................... P, FP, G .................... Cool, ≤6 °C 16 .. 36 hours 

Table lB—Inorganic Tests: 

1. Acidity ....................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 14 days 

2. Alkalinity .................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 14 days 

4. Ammonia ................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

9. Biochemical oxygen demand .................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

10. Boron ...................................................................................................................... P, FP, or Quartz ........ HNO3 to pH<2 6 months 

11. Bromide ................................................................................................................... P, FP, G .................... None required 28 days 

14. Biochemical oxygen demand, carbonaceous ......................................................... P, FP G ..................... Cool, ≤6 °C 18 .. 48 hours 

15. Chemical oxygen demand ...................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

16. Chloride ................................................................................................................... P, FP, G .................... None required 28 days 

17. Chlorine, total residual ............................................................................................ P, G ........................... None required Analyze within 15 minutes 

21. Color ....................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

23–24. Cyanide, total or available (or CATC) .............................................................. P, FP, G .................... Cool, ≤6 °C 18, 

NaOH to 

pH>12 6, reducing 

agent 5.

14 days 

25. Fluoride ................................................................................................................... P ................................ None required 28 days 

27. Hardness ................................................................................................................. P, FP, G .................... HNO3 or 

H2SO4 to 

pH<2.

6 months 

28. Hydrogen ion (pH) .................................................................................................. P, FP, G .................... None required Analyze within 15 minutes 

31, 43. Kjeldahl and organic N ..................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

Table IB—Metals: 7

18. Chromium VI ........................................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

pH = 9.3–

9.7 20.

28 days 

35. Mercury (CVAA) ...................................................................................................... P, FP, G .................... HNO3 to pH<2 28 days 


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TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued 

Parameter number/name Container 1 Preservation 2,3 Maximum holding time 4

35. Mercury (CVAFS) ................................................................................................... FP, G; and FP-lined 

cap 17.

5 mL/L 12N 

HCl or 5 mL/ 

L BrCl 17.

90 days 17

3, 5–8, 12, 13, 19, 20, 22, 26, 29, 30, 32–34, 36, 37, 45, 47, 51, 52, 58–60, 62, 63, 

70–72, 74, 75. Metals, except boron, chromium VI, and mercury.

P, FP, G .................... HNO3 to pH<2, 

or at least 24 

hours prior to 

analysis 19.

6 months 

38. Nitrate ..................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

39. Nitrate-nitrite ........................................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

40. Nitrite ....................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

41. Oil and grease ........................................................................................................ G ................................ Cool to ≤6 

°C 18, HCl or 

H2SO4 to 

pH<2.

28 days 

42. Organic Carbon ...................................................................................................... P, FP, G .................... Cool to ≤6 

°C 18, HCl, 

H2SO4, or 

H3PO4 to 

pH<2.

28 days 

44. Orthophosphate ...................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. Filter within 15 minutes; Analyze within 48 hours 

46. Oxygen, Dissolved Probe ....................................................................................... G, Bottle and top ....... None required Analyze within 15 minutes 

47. Winkler .................................................................................................................... G, Bottle and top ....... Fix on site and 

store in dark.

8 hours 

48. Phenols ................................................................................................................... G ................................ Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

49. Phosphorous (elemental) ........................................................................................ G ................................ Cool, ≤6 °C 18 .. 48 hours 

50. Phosphorous, total .................................................................................................. P, FP, G .................... Cool, ≤6 °C 18, 

H2SO4 to 

pH<2.

28 days 

53. Residue, total .......................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 7 days 

54. Residue, Filterable .................................................................................................. P, FP, G .................... Cool, ≤6 °C 18 .. 7 days 

55. Residue, Nonfilterable (TSS) .................................................................................. P, FP, G .................... Cool, ≤6 °C 18 .. 7 days 

56. Residue, Settleable ................................................................................................. P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

57. Residue, Volatile ..................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 7 days 

61. Silica ....................................................................................................................... P or Quartz ................ Cool, ≤6 °C 18 .. 28 days 

64. Specific conductance .............................................................................................. P, FP, G .................... Cool, ≤6 °C 18 .. 28 days 

65. Sulfate ..................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18 .. 28 days 

66. Sulfide ..................................................................................................................... P, FP, G .................... Cool, ≤6 °C 18, 

add zinc acetate plus sodium hydroxide to pH>9.

7 days 

67. Sulfite ...................................................................................................................... P, FP, G .................... None required Analyze within 15 minutes 

68. Surfactants .............................................................................................................. P, FP, G .................... Cool, ≤6 °C 18 .. 48 hours 

69. Temperature ........................................................................................................... P, FP, G .................... None required Analyze 

73. Turbidity .................................................................................................................. P, FP, G .................... Cool, ≤6 °C 18 48 hours 

Table lC—Organic Tests 8

13, 18–20, 22, 24–28, 34–37, 39–43, 45–47, 56, 76, 104, 105, 108–111, 113. 

Purgeable Halocarbons.

G, FP-lined septum ... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3 5.

14 days 

6, 57, 106. Purgeable aromatic hydrocarbons ............................................................. G, FP-lined septum ... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3 5, 

HCl to pH 2 9.

14 days 9

3, 4. Acrolein and acrylonitrile ...................................................................................... G, FP-lined septum ... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3 5, 

pH to 4-5 10.

14 days 10

23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112. Phenols 11 ............................................. G, FP-lined cap ......... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3 5.

7 days until extraction, 40 days 

after extraction 

7, 38. Benzidines 11, 12 .................................................................................................. G, FP-lined cap ......... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3 5.

7 days until extraction 13

14, 17, 48, 50–52. Phthalate esters 11 ......................................................................... G, FP-lined cap ......... Cool, ≤6 °C 18 .. 7 days until extraction, 40 days 

after extraction 

82–84. Nitrosamines11 14 .............................................................................................. G, FP-lined cap ......... Cool, ≤6 °C 18, 

store in dark, 

0.008% 

Na2S2O3

5.

7 days until extraction, 40 days 

after extraction 

88–94. PCBs 11 ............................................................................................................. G, FP-lined cap ......... Cool, ≤6 °C 18 .. 1 year until extraction, 1 year 

after extraction 

54, 55, 75, 79. Nitroaromatics and isophorone 11 ........................................................ G, FP-lined cap ......... Cool, ≤6 °C 18, 

store in dark, 

0.008% 

Na2S2O3

5.

7 days until extraction, 40 days 

after extraction 


rwilkins on PROD1PC63 with RULES
11238 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

TABLE II.—REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES—Continued 

Parameter number/name Container 1 Preservation 2,3 Maximum holding time 4

1, 2, 5, 8–12, 32, 33, 58, 59, 74, 78, 99, 101. Polynuclear aromatic hydrocarbons 11 G, FP-lined cap ......... Cool, ≤6 °C 18, 

store in dark, 

0.008% 

Na2S2O3

5.

7 days until extraction, 40 days 

after extraction 

15, 16, 21, 31, 87. Haloethers 11 .................................................................................. G, FP-lined cap ......... Cool, ≤6 °C 18, 

0.008% 

Na2S2O3

5.

7 days until extraction, 40 days 

after extraction 

29, 35-37, 63-65, 107. Chlorinated hydrocarbons 11 .................................................... G, FP-lined cap ......... Cool, ≤6 °C 18 .. 7 days until extraction, 40 days 

after extraction 

60-62, 66-72, 85, 86, 95-97, 102, 103. CDDs/CDFs 11.

Aqueous Samples: Field and Lab Preservation .................................................... G ................................ Cool, ≤6 °C 18, 

0.008% 

Na2S2O3

5, 

pH<9.

1 year 

Solids and Mixed-Phase Samples: Field Preservation ......................................... G ................................ Cool, ≤6 °C 18 .. 7 days 

Tissue Samples: Field Preservation ...................................................................... G ................................ Cool, ≤6 °C 18 24 hours 

Solids, Mixed-Phase, and Tissue Samples: Lab Preservation ............................. G ................................ Freeze, ≤¥10 

°C.

1 year 

Table lD—Pesticides Tests: 

1–70. Pesticides 11 ........................................................................................................ G, FP-lined cap ......... Cool, ≤6 °C 18, 

pH 5–9 15.

7 days until extraction, 40 days 

after extraction 

Table lE—Radiological Tests: 

1–5. Alpha, beta, and radium ....................................................................................... P, FP, G .................... HNO3 to pH<2 6 months 

1 ‘‘P’’ is 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 sterlizable material (polypropylene or other autoclavable plastic); ‘‘LDPE’’ is low density polyethylene. 2Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15 minutes of collection. For a composite sample collected with an automated 

sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at ≤6 °C during collection unless specified otherwise 

in this Table II or in the method(s). For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at ≤6 °C, unless specified otherwise in this 

Table II or in the method(s), until collection, splitting, and preservation is completed. Add the preservative to the sample container prior to sample collection when the preservative will not 

compromise the integrity of a grab sample, a composite sample, or an aliquot split from a composite sample ; otherwise, preserve the grab sample, composite sample, or aliquot split from a 

composite sample with in 15 minutes of collection. If a composite measurement is required but a composite sample would compromise sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations averaged. Alternatively, 

grab samples may be collected in the field and composited in the laboratory if the compositing procedure produces results equivalent to results produced by arithmetic averaging of the results of analysis of individual grab samples. For examples of laboratory compositing procedures, see EPA Method 1664A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and 

(v) (volatile organics). 3When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with the Department of Transportation Hazardous Materials Regulations (49 

CFR Part 172). The person offering such material for transportation is responsible for ensuring such compliance. For the preservation requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCl) 

in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 

or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or less). 4Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples may be held before the start of analysis and still be considered 

valid (e.g., samples analyzed for fecal coliforms may be held up to 6 hours prior to commencing analysis). Samples may be held for longer periods only if the permittee or monitoring laboratory has data on file to show that, for the specific types of samples under study, the analytes are stable for the longer time, and has received a variance from the Regional Administrator 

under § 136.3(e). For a grab sample, the holding time begins at the time of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; 

see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), the holding time begins at the time of the end of collection of the composite sample. For a set of grab samples composited in 

the field or laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples may not be stable for the maximum time period given in the table. A 

permittee or monitoring laboratory is obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain sample stability. See § 136.3(e) for details. The 

date and time of collection of an individual grab sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and that are all collected on the 

same calendar date, the date of collection is the date on which the samples are collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the 

date of collection is the dates of the two days; e.g., November 14–15. For a composite sample collected automatically on a given date, the date of collection is the date on which the sample 

is collected. For a composite sample collected automatically, and that is collected across two calendar dates, the date of collection is the dates of the two days; e.g., November 14–15. 5Add a reducing agent only if an oxidant (e.g., chlorine) is present. Reducing agents shown to be effective are sodium thiosulfate (Na2S2O3), ascorbic acid, sodium arsenite (NaAsO2), or 

sodium borohydride (NaBH4). However, some of these agents have been shown to produce a positive or negative cyanide bias, depending on other substances in the sample and the analytical method used. Therefore, do not add an excess of reducing agent. Methods recommending ascorbic acid (e.g., EPA Method 335.4) specify adding ascorbic acid crystals, 0.1—0.6 g, until 

a drop of sample produces no color on potassium iodide (KI) starch paper, then adding 0.06 g (60 mg) for each liter of sample volume. If NaBH4 or NaAsO2 is used, 25 mg/L NaBH4 or 100 

mg/L NaAsO2 will reduce more than 50 mg/L of chlorine (see method (Kelada-01’’ and/or Standard Method 4500-CN¥ for more information). After adding reducing agent, test the sample 

using KI paper, a test strip (e.g. for chlorine, SenSafeTM Total Chlorine Water Check 480010) moistened with acetate buffer solution (see Standard Method 4500-Cl.C.3e), or a chlorine/oxidant test method (e.g., EPA Method 330.4 or 330.5), to make sure all oxidant is removed. If oxidant remains, add more reducing agent. Whatever agent is used, it should be tested to assure 

that cyanide results are not affected adversely. 6Sample collection and preservation: Collect a volume of sample appropriate to the analytical method in a bottle of the material specified. If the sample can be analyzed within 48 hours 

and sulfide is not present, adjust the pH to >12 with sodium hydroxide solution (e.g., 5 % w/v), refrigerate as specified, and analyze within 48 hours. Otherwise, to extend the holding time to 

14 days and mitigate interferences, treat the sample immediately using any or all of the following techniques, as necessary, followed by adjustment of the sample pH to >12 and refrigeration 

as specified. There may be interferences that are not mitigated by approved procedures. Any procedure for removal or suppression of an interference may be employed, provided the laboratory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g., ferric ferrocyanide) or a strong cyanide complex (e.g., cobalt cyanide) are more accurately measured if 

the laboratory holds the sample at room temperature and pH >12 for a minimum of 4 hours prior to analysis, and performs UV digestion or dissolution under alkaline (pH=12) conditions, if 

necessary. 

(1) Sulfur: To remove elemental sulfur (S8), filter the sample immediately. If the filtration time will exceed 15 minutes, use a larger filter or a method that requires a smaller sample volume 

(e.g., EPA Method 335.4 or Lachat Method 01). Adjust the pH of the filtrate to >12 with NaOH, refrigerate the filter and filtrate, and ship or transport to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the 

pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate 

from the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in μg or mg), and divide by the original sample volume to obtain 

the cyanide concentration. 

(2) Sulfide: If the sample contains sulfide as determined by lead acetate paper, or if sulfide is known or suspected to be present, immediately conduct one of the volatilization treatments or 

the precipitation treatment as follows: Volatilization—Headspace expelling. In a fume hood or well-ventilated area, transfer 0.75 liter of sample to a 4.4-L collapsible container (e.g., 

CubitainerTM). Acidify with concentrated hydrochloric acid to pH <2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel the headspace into the fume hood or 

open area by collapsing the container without expelling the sample. Refill the headspace by expanding the container. Repeat expelling a total of five headspace volumes. Adjust the pH to 

>12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio. A larger volume of air will result in too 

great a loss of cyanide (> 10%). Dynamic stripping: In a fume hood or well-ventilated area, transfer 0.75 liter of sample to a container of the material specified and acidify with concentrated 

hydrochloric acid to pH <2. Using a calibrated air sampling pump or flowmeter, purge the acidified sample into the fume hood or open area through a fritted glass aerator at a flow rate of 

2.25 L/min for 4 minutes. Adjust the pH to >12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio. 

A larger volume of air will result in too great a loss of cyanide (>10%). Precipitation: If the sample contains particulate matter that would be removed by filtration, filter the sample prior to 

treatment to assure that cyanide associated with the particulate matter is included in the measurement. Ship or transport the filter to the laboratory. In the laboratory, extract the filter with 100 

mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to approximately 12 

with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the 

sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in μg or mg), and divide by the original sample volume to obtain the cyanide concentration. For removal of sulfide by precipitation, raise the pH of the sample to >12 with NaOH solution, then add approximately 1 mg of powdered cadmium chloride for each mL of sample. For 

example, add approximately 500 mg to a 500-mL sample. Cap and shake the container to mix. Allow the precipitate to settle and test the sample with lead acetate paper. If necessary, add 

cadmium chloride but avoid adding an excess. Finally, filter through 0.45 micron filter. Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, 

lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the 

filtrate form the solids, test the sample with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined (in (g or mg), and divide by the original sample volume to 

obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM D6888), it may be necessary to increase the ligand-exchange reagent to offset any excess of cadmium 

chloride. 

(3) Sulfite, thiosulfate, or thiocyanate: If sulfite, thiosulfate, or thiocyanate is known or suspected to be present, use UV digestion with a glass coil (Method Kelada-01) or ligand exchange 

(Method OIA–1677) to preclude cyanide loss or positive interference. 


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(4) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be present, treat the sample with 20 mL of 3.5% ethylenediamine solution per liter 

of sample. 

(5) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the distillation flask, a reduction in the pH of the absorber solution, and incomplete cyanide spike recovery. When significant carbonate is present, adjust the pH to ≥ 12 using calcium hydroxide instead of sodium hydroxide. Allow the precipitate to settle and decant or filter the 

sample prior to analysis (also see Standard Method 4500-CN.B.3.d). 

(6) Chlorine, hypochlorite, or other oxidant: Treat a sample known or suspected to contain chlorine, hypochlorite, or other oxidant as directed in footnote 5. 7For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives. For a composite sample collected with an automated sampler (e.g., using a 24- 

hour composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of collection and before adding preservatives. If it 

is known or suspected that dissolved sample integrity will be compromised during collection of a composite sample collected automatically over time (e.g., by interchange of a metal between 

dissolved and suspended forms), collect and filter grab samples to be composited (footnote 2) in place of a composite sample collected automatically. 8Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds. 

9 If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling. 

10The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling. 11When the extractable analytes of concern fall within a single chemical category, the specified preservative and maximum holding times should be observed for optimum safeguard of 

sample integrity (i.e., use all necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two or more chemical categories, the sample may be preserved by cooling to ≤6 °C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this manner may be held for 

seven days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for 

thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine). 12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ± 0.2 to prevent rearrangement to benzidine. 13Extracts may be stored up to 30 days at <0 °C. 14For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7–10 with NaOH within 24 hours of sampling. 15The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 

0.008% Na2S2O3. 16Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still present when the samples arrive at the laboratory. However, even if ice is present 

when the samples arrive, it is necessary to immediately measure the temperature of the samples and confirm that the preservation temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance. The request for a 

variance should include supportive data which show that the toxicity of the effluent samples is not reduced because of the increased holding temperature. 17Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved with 

BrCl or HCl solution within 48 hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the sample bottle. A sample collected for dissolved 

trace level mercury should be filtered in the laboratory within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample should be filtered in a 

designated clean area in the field in accordance with procedures given in Method 1669. If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample 

must be filtered in a designated clean area in the field within the time period necessary to maintain sample integrity. A sample that has been collected for determination of total or dissolved 

trace level mercury must be analyzed within 90 days of sample collection. 18Aqueous samples must be preserved at ≤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 of NPDES monitoring, the specification of ‘‘≤ °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 (1/100th of 1 degree); rather, three significant figures are specified so that 

rounding down to 6 °C may not be used to meet the ≤6 °C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less than 15 minutes). 19An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at least 24 hours before analysis to dissolve any metals that adsorb to the 

container walls. If the sample must be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment samples do not need to be preserved with acid. 

The allowances in this footnote supersede the preservation and holding time requirements in the approved metals methods. 20To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6. The allowance in this footnote supersedes preservation and holding time 

requirements in the approved hexavalent chromium methods, unless this supersession would compromise the measurement, in which case requirements in the method must be followed. 21 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in bulk and calculated from the time of sample filtration to elution for samples filtered in the field. 

■ 8. Section 136.4 is amended by 

revising the first sentence of paragraph 

(d) introductory text to read as follows: 

§ 136.4 Application for alternate test 

procedures. 

* * * * * 

(d) An application for approval of an 

alternate test procedure for nationwide 

use may be made by letter in triplicate 

to the Alternate Test Procedure Program 

Coordinator, Office of Science and 

Technology (4303), Office of Water, U.S. 

Environmental Protection Agency, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460. * * * 

* * * * * 

■ 9. Section 136.5 is amended as 

follows: 

■ a. In paragraph (b) by revising the last 

sentence. 

■ b. By revising paragraph (c). 

■ c. In paragraph (d) by revising the 

second and third sentences. 

■ d. By revising paragraphs (e)(1) and 

(e)(2). 

§ 136.5 Approval of alternate test 

procedures. 

* * * * * 

(b) * * * Where the Director 

recommends rejection of the application 

for scientific and technical reasons 

which he provides, the Regional 

Administrator shall deny the 

application and shall forward this 

decision to the Director of the State 

Permit Program and to the Alternate 

Test Procedure Program Coordinator, 

Office of Science and Technology 

(4303), Office of Water, U.S. 

Environmental Protection Agency, 1200 

Pennsylvania Ave., NW., Washington, 

DC 20460. 

(c) Before approving any application 

for an alternate test procedure proposed 

by the responsible person or firm 

making the discharge, the Regional 

Administrator shall forward a copy of 

the application to the Alternate Test 

Procedure Program Coordinator, Office 

of Science and Technology (4303), 

Office of Water, U.S. Environmental 

Protection Agency, 1200 Pennsylvania 

Ave., NW., Washington, DC 20460. 

(d) * * * Prior to the expiration of 

such ninety day period, a 

recommendation providing the 

scientific and other technical basis for 

acceptance or rejection will be 

forwarded to the Regional Administrator 

by the Alternate Test Procedure Program 

Coordinator, Washington, DC. A copy of 

all approval and rejection notifications 

will be forwarded to the Alternate Test 

Procedure Program Coordinator, Office 

of Science and Technology (4303), 

Office of Water, U.S. Environmental 

Protection Agency, 1200 Pennsylvania 

Ave., NW., Washington, DC 20460, for 

the purposes of national coordination. 

(e) Approval for nationwide use. (1) 

As expeditiously as is practicable after 

receipt by the Alternate Test Procedure 

Program Coordinator, Washington, DC, 

of an application for an alternate test 

procedure for nationwide use, the 

Alternate Test Procedure Program 

Coordinator, Washington, DC, shall 

notify the applicant in writing whether 

the application is complete. If the 

application is incomplete, the applicant 

shall be informed of the information 

necessary to make the application 

complete. 

(2) As expeditiously as is practicable 

after receipt of a complete package, the 

Alternate Test Procedure Program 

Coordinator shall perform any analysis 

necessary to determine whether the 

alternate test procedure satisfies the 

applicable requirements of this part, and 

the Alternate Test Procedure Program 

Coordinator shall recommend to the 

Administrator that he/she approve or 

reject the application and shall also 

notify the application of the 

recommendation. 

* * * * * 

■ 10. Section 136.6 is added to Part 136 

to read as follows: 

§ 136.6 Method Modifications and 

Analytical Requirements. 

(a) Definitions of terms used in this 

Section. 

(1) Analyst means the person or 

laboratory using a test procedure 

(analytical method) in this Part. 

(2) Chemistry of the Method means 

the reagents and reactions used in a test 

procedure that allow determination of 

the analyte(s) of interest in an 

environmental sample. 

(3) Determinative Technique means 

the way in which an analyte is 

identified and quantified (e.g., 

colorimetry, mass spectrometry). 

(4) Equivalent Performance means 

that the modified method produces 

results that meet the QC acceptance 


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criteria of the approved method at this 

part. 

(5) Method-defined Analyte means an 

analyte defined solely by the method 

used to determine the analyte. Such an 

analyte may be a physical parameter, a 

parameter that is not a specific 

chemical, or a parameter that may be 

comprised of a number of substances. 

Examples of such analytes include 

temperature, oil and grease, total 

suspended solids, total phenolics, 

turbidity, chemical oxygen demand, and 

biochemical oxygen demand. 

(6) QC means ‘‘quality control.’’

(b) Method Modifications. 

(1) Allowable Changes. Except as set 

forth in paragraph (b)(3) of this section, 

an analyst may modify an approved test 

procedure (analytical method) provided 

that the chemistry of the method or the 

determinative technique is not changed, 

and provided that the requirements of 

paragraph (b)(2) of this section are met. 

(i) Potentially acceptable 

modifications regardless of current 

method performance include changes 

between automated and manual discrete 

instrumentation; changes in the 

calibration range (provided that the 

modified range covers any relevant 

regulatory limit); changes in equipment 

such as using similar equipment from a 

vendor other than that mentioned in the 

method (e.g., a purge-and-trap device 

from OIA rather than Tekmar), changes 

in equipment operating parameters such 

as changing the monitoring wavelength 

of a colorimeter or modifying the 

temperature program for a specific GC 

column; changes to chromatographic 

columns (treated in greater detail in 

paragraph (d) of this section); and 

increases in purge-and-trap sample 

volumes (provided specifications in 

paragraph (e) of this section are met). 

The changes are only allowed provided 

that all the requirements of paragraph 

(b)(2) of this section are met. 

(ii) If the characteristics of a 

wastewater matrix prevent efficient 

recovery of organic pollutants and 

prevent the method from meeting QC 

requirements, the analyst may attempt 

to resolve the issue by using salts as 

specified in Guidance on Evaluation, 

Resolution, and Documentation of 

Analytical Problems Associated with 

Compliance Monitoring (EPA 821–B–

93–001, June 1993), provided that such 

salts do not react with or introduce the 

target pollutant into the sample (as 

evidenced by the analysis of method 

blanks, laboratory control samples, and 

spiked samples that also contain such 

salts) and that all requirements of 

paragraph (b)(2) of this section are met. 

Chlorinated samples must be 

dechlorinated prior to the addition of 

such salts. 

(iii) If the characteristics of a 

wastewater matrix result in poor sample 

dispersion or reagent deposition on 

equipment and prevents the analyst 

from meeting QC requirements, the 

analysts may attempt to resolve the 

issue by adding an inert surfactant (i.e. 

a surfactant that will not affect the 

chemistry of the method), which may 

include Brij-35 or sodium dodecyl 

sulfate (SDS), provided that such 

surfactant does not react with or 

introduce the target pollutant into the 

sample (as evidenced by the analysis of 

method blanks, laboratory control 

samples, and spiked samples that also 

contain such surfactant) and that all 

requirements of paragraph (b)(2) of this 

section are met. Chlorinated samples 

must be dechlorinated prior to the 

addition of such surfactant. 

(2) Requirements. A modified method 

must produce equivalent performance to 

the approved methods for the analyte(s) 

of interest, and the equivalent 

performance must be documented. 

(i) Requirements for Establishing 

Equivalent Performance 

(A) If the approved method contains 

QC tests and QC acceptance criteria, the 

modified method must use these QC 

tests and the modified method must 

meet the QC acceptance criteria. The 

Analyst may only rely on QC tests and 

QC acceptance criteria in a method if it 

includes wastewater matrix QC tests 

and QC acceptance criteria (e.g., as 

matrix spikes) and both initial (start-up) 

and ongoing QC tests and QC 

acceptance criteria. 

(B) If the approved method does not 

contain QC tests and QC acceptance 

criteria, or if the QC tests and QC 

acceptance criteria in the method do not 

meet the requirements of paragraph 

(b)(2)(i)(A) of this section, the analyst 

must employ QC tests specified in 

Protocol for EPA Approval of Alternate 

Test Procedures for Organic and 

Inorganic Analytes in Wastewater and 

Drinking Water (EPA–821–B–98–002, 

March 1999) and meet the QC 

provisions specified therein. In 

addition, the Analyst must perform ongoing QC tests, including assessment of 

performance of the modified method on 

the sample matrix (e.g., analysis of a 

matrix spike/matrix spike duplicate pair 

for every twenty samples of a discharge 

analyzed), and analysis of an ongoing 

precision and recovery sample and a 

blank with each batch of 20 or fewer 

samples. 

(C) Calibration must be performed 

using the modified method and the 

modified method must be tested with 

every wastewater matrix to which it will 

be applied (up to nine distinct matrices; 

as described in the ATP Protocol, after 

validation in nine distinct matrices, the 

method may be applied to all 

wastewater matrices), in addition to any 

and all reagent water tests. If the 

performance in the wastewater matrix or 

reagent water does not meet the QC 

acceptance criteria the method 

modification may not be used. 

(D) Analysts must test representative 

effluents with the modified method, and 

demonstrate that the results are 

equivalent or superior to results with 

the unmodified method. 

(ii) Requirements for Documentation. 

The modified method must be 

documented in a method write-up or an 

addendum that describes the 

modification(s) to the approved method. 

The write-up or addendum must 

include a reference number (e.g., 

method number), revision number, and 

revision date so that it may be 

referenced accurately. In addition, the 

organization that uses the modified 

method must document the results of 

QC tests and keep these records, along 

with a copy of the method write-up or 

addendum, for review by an auditor. 

(3) Restrictions. An analyst may not 

modify an approved analytical method 

for a method-defined analyte. In 

addition, an analyst may not modify an 

approved method if the modification 

would result in measurement of a 

different form or species of an analyte 

(e.g., a change to a metals digestion or 

total cyanide distillation). An analyst 

may also may not modify any sample 

preservation and/or holding time 

requirements of an approved method. 

(c) Analytical Requirements for Multianalyte Methods (Target Analytes). For 

the purpose of NPDES reporting, the 

discharger or permittee must meet QC 

requirements only for the analyte(s) 

being measured and reported under the 

NPDES permit. 

(d) The following modifications to 

approved methods are authorized in the 

circumstances described below: 

(1) Capillary Column. Use of a 

capillary (open tubular) GC column 

rather than a packed column is allowed 

with EPA Methods 601–613, 624, 625, 

and 1624B in Appendix A to this part, 

provided that all QC tests for the 

approved method are performed and all 

QC acceptance criteria are met. When 

changing from a packed column to a 

capillary column, retention times will 

change. Analysts are not required to 

meet retention time specified in the 

approved method when this change is 

made. Instead, analysts must generate 

new retention time tables with capillary 

columns to be kept on file along with 


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other startup test and ongoing QC data, 

for review by auditors. 

(2) Increased sample volume in purge 

and trap methodology. Use of increased 

sample volumes, up to a maximum of 25 

mL, is allowed for an approved method, 

provided that the height of the water 

column in the purge vessel is at least 5 

cm. The analyst should also use one or 

more surrogate analytes that are 

chemically similar to the analytes of 

interest in order to demonstrate that the 

increased sample volume does not 

adversely affect the analytical results. 

PART 141—NATIONAL PRIMARY 

DRINKING WATER REGULATIONS 

■ 11. The authority citation for part 141 

continues to read as follows: 

Authority: 42 U.S.C. 300f, 300g–1, 300g–2, 

300g–3, 300g–4, 300g–5, 300g–6, 300j–4, 

300j–9, and 300j–11. 

■ 12. Section 141.21 is amended by 

adding four sentences to the end of 

footnote 1 to the Table in paragraph 

(f)(3) to read as follows: 

§ 141.21 Coliform sampling. 

* * * * * 

(f) * * * 

(3) * * * 

1* * * In addition, the following 

online versions may also be used: 9221 

A, B, D–99, 9222 A, B, C–97, and 9223 

B–97. Standard Methods Online are 

available at http:// 

www.standardmethods.org. The year in 

which each method was approved by 

the Standard Methods Committee is 

designated by the last two digits in the 

method number. The methods listed are 

the only Online versions that may be 

used. 

* * * * * 

■ 13. Section 141.23 is amended as 

follows: 

■ a. In paragraph (a)(4)(i) by revising the 

table entries for ‘‘Cyanide,’’ ‘‘Nitrate,’’

and ‘‘Nitrite’’. 

■ b. In paragraph (k)(1) by revising the 

table. 

§ 141.23 Inorganic chemical sampling and 

analytical requirements. 

* * * * * 

(a) * * * 

(4) * * * 

(i) * * * 

DETECTION LIMITS FOR INORGANIC CONTAMINANTS

Contaminant MCL (mg/L) Methodology Detection Limit (mg/L) 

* * * * * * * 

Cyanide ..................... 0.2 Distillation, Spectrophotometric3 ........................................................... 0 .02 

Distillation, Automated, Spectrophotometric3 ....................................... 0 .005 

Distillation, Amenable, Spectrophotometric4 ........................................ 0 .02 

Distillation, Selective Electrode3, 4 ........................................................ 0 .05 

UV, Distillation, Spectrophotometric9 .................................................... 0 .0005 

Micro Distillation, Flow Injection, Spectrophotometric3 ........................ 0 .0006 

Ligand Exchange with Amperometry4 .................................................. 0 .0005 

* * * * * * * 

Nitrate ........................ 10 (as N) Manual Cadmium Reduction ................................................................ 0 .01 

Automated Hydrazine Reduction .......................................................... 0 .01 

Automated Cadmium Reduction ........................................................... 0 .05 

Ion Selective Electrode ......................................................................... 1 

Ion Chromatography ............................................................................. 0 .01 

Capillary Ion Electrophoresis ................................................................ 0 .076 

Nitrite ......................... 1 (as N) Spectrophotometric ............................................................................... 0 .01 

Automated Cadmium Reduction ........................................................... 0 .05 

Manual Cadmium Reduction ................................................................ 0 .01 

Ion Chromatography ............................................................................. 0 .004 

Capillary Ion Electrophoresis ................................................................ 0 .103 

* * * * * * * 

* * * * * 

3 Screening method for total cyanides. 4 Measures ‘‘free’’ cyanides when distillation, digestion, or ligand exchange is omitted. 

* * * * * 

9 Measures total cyanides when UV-digestor is used, and ‘‘free’’ cyanides when UV-digestor is bypassed. 

* * * * * 

(k) * * * (1) * * * 

Contaminant Methodology 13 EPA ASTM 3 SM 4 (18th, 19th 

ed.) SM 4 (20th ed.) SM Online 22 Other 

1. Alkalinity .............. Titrimetric ........................ .................... D1067–92, 02 B ............. 2320 B ............. 2320 B ............. 2320 B–97 .......

Electrometric titration ...... .................... ......................................... ......................... ......................... I–1030–85 5.

2. Antimony .............. Inductively Coupled Plasma (ICP)—Mass Spectrometry.

200.8 2

Hydride-Atomic Absorption..................... D3697–92, 02.

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... ......................................... 3113 B ............. ......................... 3113 B–99 .......

3. Arsenic 14 ............. Inductively Coupled Plasma 15.

200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP-Mass Spectrometry 200.8 2


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Contaminant Methodology 13 EPA ASTM 3 SM 4 (18th, 19th 

ed.) SM 4 (20th ed.) SM Online 22 Other 

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... D2972–97, 03 C ............. 3113 B ............. ......................... 3113 B–99.

Hydride Atomic Absorption..................... D2972–97, 03 B ............. 3114 B ............. ......................... 3114 B–97.

4. Asbestos .............. Transmission Electron 

Microscopy.

100.1 9

Transmission Electron 

Microscopy.

100.2 10

5. Barium ................. Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP-Mass Spectrometry 200.8 2

Atomic Absorption; Direct .................... ......................................... 3111D .............. ......................... 3111 D–99.

Atomic Absorption; Furnace..................... ......................................... 3113 B ............. ......................... 3113 B–99.

6. Beryllium .............. Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP-Mass Spectrometry 200.8 2

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... D3645–97, 03 B ............. 3113 B ............. ......................... 3113 B–99.

7. Cadmium ............. Inductively Coupled Plasma.200.7 2

ICP-Mass Spectrometry 200.8 2

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... ......................................... 3113 B ............. ......................... 3113 B–99.

8. Calcium ................ EDTA titrimetric .............. .................... D511–93, 03 A ............... 3500–Ca D ...... 3500–Ca B ...... 3500–Ca B–97.

Atomic Absorption; Direct 

Aspiration.

.................... D511–93, 03 B ............... 3111 B ............. ......................... 3111 B–99.

Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

Ion Chromatography ....... .................... D6919–03.

9. Chromium ............ Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP-Mass Spectrometry 200.8 2

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... ......................................... 3113 B ............. ......................... 3113 B–99.

10. Copper ............... Atomic Absorption; Furnace..................... D1688–95, 02 C ............. 3113 B ............. ......................... 3113 B–99.

Atomic Absorption; Direct 

Aspiration.

.................... D1688–95, 02 A ............. 3111 B ............. ......................... 3111 B–99.

Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP-Mass spectrometry .. 200.8 2

Atomic Absorption; Platform.200.9 2

11. Conductivity ....... Conductance .................. .................... D1125–95 (Reapproved 

1999) A.

2510 B ............. 2510 B ............. 2510 B–97.

12. Cyanide ............. Manual Distillation followed by .................... D2036–98 A ................... 4500–CN¥ C .. 4500–CN¥ C.

Spectrophotometric, 

Amenable.

.................... D2036–98 B ................... 4500–CN¥ G .. 4500–CN¥ G .. 4500–CN¥ G–

99.

Spectro-photometric 

Manual.

.................... D2036–98 A ................... 4500–CN¥ E ... 4500–CN¥ E ... 4500–CN¥ E–

99.

I–3300–85 5

Spectro-photometric 

Semi-automated.

335.4 6

Selective Electrode ......... .................... ......................................... 4500–CN¥ F ... 4500–CN¥ F ... 4500–CN¥ F–

99.

UV, Distillation, 

Spectrophotometric.

.................... ......................................... ......................... ......................... ......................... Kelada–01 17

Micro Distillation, Flow 

Injection, 

Spectrophotometric.

.................... ......................................... ......................... ......................... ......................... QuikChem 10–

204–00–1–

X18

Ligand Exchange and 

Amperometry 21.

.................... D6888–04 ....................... ......................... ......................... ......................... OIA–1677, 

DW 20

13. Fluoride .............. Ion Chromatography ....... 300.0 6, 

300.1 19

D4327–97, 03 ................. 4110 B ............. 4110 B ............. 4110 B–00.

Manual Distill.; Color. 

SPADNS.

.................... ......................................... 4500–F¥ B, D 4500–F¥ B, D 4500–F¥ B, D–

97.

Manual Electrode ........... .................... D1179–93, 99 B ............. 4500–F¥ C ..... 4500–F¥ C ..... 4500–F¥ C–97.

Automated Electrode ...... .................... ......................................... ......................... ......................... ......................... 380–75WE11

Automated Alizarin ......... .................... ......................................... 4500–F¥ E ...... 4500–F¥ E ...... 4500–F¥ E–97 129–71W 11

Capillary Ion Electrophoresis..................... ......................................... ......................... ......................... ......................... D6508, Rev. 

2 23

14. Lead ................... Atomic Absorption; Furnace..................... D3559–96, 03 D ............. 3113 B ............. ......................... 3113 B–99.

ICP–Mass spectrometry 200.8 2


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11243 

Contaminant Methodology 13 EPA ASTM 3 SM 4 (18th, 19th 

ed.) SM 4 (20th ed.) SM Online 22 Other 

Atomic Absorption; Platform.200.9 2

Differential Pulse Anodic 

Stripping Voltametry.

.................... ......................................... ......................... ......................... ......................... Method 1001 16

15. Magnesium ........ Atomic Absorption .......... .................... D511–93, 03 B ............... 3111 B ............. ......................... 3111 B–99.

ICP .................................. 200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

Complexation Titrimetric 

Methods.

.................... D511–93, 03 A ............... 3500–Mg E ...... 3500–Mg B ...... 3500–Mg B–97.

Ion Chromatography ....... .................... D6919–03.

16. Mercury .............. Manual, Cold Vapor ....... 245.1 2 ........ D3223–97, 02 ................. 3112 B ............. ......................... 3112 B–99.

Automated, Cold Vapor .. 245.2 1

ICP–Mass Spectrometry 200.8 2

17. Nickel ................. Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

ICP–Mass Spectrometry 200.8 2

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Direct .................... ......................................... 3111 B ............. ......................... 3111 B–99.

Atomic Absorption; Furnace..................... ......................................... 3113 B ............. ......................... 3113 B–99.

18. Nitrate ................ Ion Chromatography ....... 300.0 6

300.1 19

D4327–97, 03 ................. 4110 B ............. 4110 B ............. 4110 B–00 ....... B–1011 8

Automated Cadmium Reduction.353.2 6 ........ D3867–90 A ................... 4500–NO3

¥ F 4500–NO3¥ F 4500–NO3¥ F–

00.

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

¥ D 4500–NO3¥ D 4500–NO3¥ D–

00.

601 7

Manual Cadmium Reduction..................... D3867–90 B ................... 4500–NO3

¥ E 4500–NO3¥ E 4500–NO3¥ E–

00.

Capillary Ion Electrophoresis..................... ......................................... ......................... ......................... ......................... D6508, Rev. 

2 23

19. Nitrite ................. Ion Chromatography ....... 300.0 6

300.1 19

D4327–97, 03 ................. 4110 B ............. 4110 B ............. 4110 B–00 ....... B–1011 8

Automated Cadmium Reduction.353.2 6 ........ D3867–90 A ................... 4500–NO3

¥ F 4500–NO3¥ F 4500–NO3¥ F–

00.

Manual Cadmium Reduction..................... D3867–90 B ................... 4500–NO3

¥ E 4500–NO3¥ E 4500–NO3¥ E–

00.

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

¥ B 4500–NO2¥ B 4500–NO2¥ B–

00.

Capillary Ion Electrophoresis..................... ......................................... ......................... ......................... ......................... D6508, Rev. 

2 23

20. Ortho-phosphate 12.

Colorimetric, Automated, 

Ascorbic Acid.

365.1 6 ........ ......................................... 4500–P F ........ 4500–P F.

Colorimetric, ascorbic 

acid, single reagent.

.................... D515–88 A ..................... 4500–P E ........ 4500–P E.

Colorimetric 

Phosphomolybdate; 

.................... ......................................... ......................... ......................... ......................... I–1601–85 5

Automated-segmented flow; .................... ......................................... ......................... ......................... ......................... I–2601–90 5

Automated Discrete .................... ......................................... ......................... ......................... ......................... I–2598–85 5

Ion Chromatography ....... 300.0 6 ........

300.1 19 ......

D4327–97, 03 ................. 4110 B ............. 4110 B ............. 4110 B–00.

Capillary Ion Electrophoresis..................... ......................................... ......................... ......................... ......................... D6508, Rev. 

2 23

21. pH ...................... Electrometric ................... 150.1, 

150.2 1

D1293–95, 99 ................. 4500–H∂ B ..... 4500–H∂ B ..... 4500–H∂ B–00.

22. Selenium ............ Hydride-Atomic Absorption..................... D3859–98, 03 A ............. 3114 B ............. ......................... 3114 B–97.

ICP–Mass Spectrometry 200.8 2

Atomic Absorption; Platform.200.9 2

Atomic Absorption; Furnace..................... D3859–98, 03 B ............. 3113 B ............. ......................... 3113 B–99.

23. Silica .................. Colorimetric, Molybdate 

Blue.

.................... ......................................... ......................... ......................... ......................... I–1700–85 5

Automated-segmented Flow..................... ......................................... ......................... ......................... ......................... I–2700–85 5

Colorimetric .................... .................... D859–94, 00.

Molybdosilicate ............... .................... ......................................... 4500–Si D ....... 4500–SiO2 C ... 4500–SiO2 C–

97.

Heteropoly blue .............. .................... ......................................... 4500–Si E ....... 4500–SiO2 D ... 4500–SiO2 D–

97.

Automated for Molybdate-reactive Silica..................... ......................................... 4500–Si F ........ 4500–SiO2 E ... 4500–SiO2 E–

97.

Inductively Coupled Plasma.200.7 2 ........ ......................................... 3120 B ............. 3120 B ............. 3120 B–99.

24. Sodium .............. Inductively Coupled Plasma.200.7 2

Atomic Absorption; Direct 

Aspiration.

.................... ......................................... 3111 B ............. ......................... 3111 B–99.

Ion Chromatography ....... .................... D6919–03.

25. Temperature ...... Thermometric ................. .................... ......................................... 2550 ................ 2550 ................ 2550–00.

26. Thallium ............. ICP–Mass Spectrometry 200.8 2


rwilkins on PROD1PC63 with RULES
11244 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

Contaminant Methodology 13 EPA ASTM 3 SM 4 (18th, 19th 

ed.) SM 4 (20th ed.) SM Online 22 Other 

Atomic Absorption; Platform.200.9 2.

The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents listed in footnotes 1–11, 16–20, and 22–23 was 

approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800–426–4791. Documents may be inspected at EPA’s Drinking Water Docket, EPA West, 

1301 Constitution Avenue, NW., Room 3334, Washington, DC 20460 (Telephone: 202–566–2426); or at the National Archives and Records Administration (NARA). For information on the 

availability of this material at NARA, call 202–741–6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. 1 ‘‘Methods for Chemical Analysis of Water and Wastes,’’ EPA/600/4–79/020, March 1983. Available at NTIS, PB84–128677. 2 ‘‘Methods for the Determination of Metals in Environmental Samples—Supplement I,’’ EPA/600/R–94/111, May 1994. Available at NTIS, PB95–125472. 3Annual Book of ASTM Standards, 1994, 1996, 1999, or 2003, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. The previous 

versions of D1688–95A, D1688–95C (copper), D3559–95D (lead), D1293–95 (pH), D1125–91A (conductivity) and D859–94 (silica) are also approved. These previous versions D1688–90A, C; 

D3559–90D, D1293–84, D1125–91A and D859–88, respectively are located in the Annual Book of ASTM Standards, 1994, Vol. 11.01. Copies may be obtained from ASTM International, 100 

Barr Harbor Drive, West Conshohocken, PA 19428. 4Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American Public Health Association, 1015 Fifteenth 

Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except that the versions of 3111 B, 3111 D, 3113 B and 3114 B in the 20th 

edition may not be used. 5 Method I–2601–90, Methods for Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial 

Sediment, Open File Report 93–125, 1993; For Methods I–1030–85; I–1601–85; I–1700–85; I–2598–85; I–2700–85; and I–3300–85 See Techniques of Water Resources Investigation of the 

U.S. Geological Survey, Book 5, Chapter A–1, 3rd edition., 1989; Available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, CO 80225–0425. 6 ‘‘Methods for the Determination of Inorganic Substances in Environmental Samples,’’ EPA/600/R–93/100, August 1993. Available at NTIS, PB94–120821. 7The procedure shall be done in accordance with the Technical Bulletin 601 ’’ Standard Method of Test for Nitrate in Drinking Water,’’ July 1994, PN 221890–001, Analytical Technology, 

Inc. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129. 8 Method B–1011, ‘‘Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography,’’ August 1987. Copies may be obtained from Waters Corporation, Technical Services Division, 34 Maple Street, Milford, MA 01757, Telephone: 508/482–2131, Fax: 508/482–3625. 9 Method 100.1, ‘‘Analytical Method For Determination of Asbestos Fibers in Water,’’ EPA/600/4–83/043, EPA, September 1983. Available at NTIS, PB83–260471. 10 Method 100.2, ‘‘Determination of Asbestos Structure Over 10-μm In Length In Drinking Water,’’ EPA/600/R–94/134, June 1994. Available at NTIS, PB94–201902. 11 Industrial Method No. 129–71W, ‘‘Fluoride in Water and Wastewater,’’ December 1972, and Method No. 380–75WE, ‘‘Fluoride in Water and Wastewater,’’ February 1976, Technicon Industrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089. 12 Unfiltered, no digestion or hydrolysis. 13Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2x preconcentration step during sample digestion, MDLs determined when samples are analyzed by 

direct analysis (i.e., no sample digestion) will be higher. For direct analysis of cadmium and arsenic by Method 200.7, and arsenic by Method 3120 B, sample preconcentration using pneumatic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and 

lead by Method 3113 B; and lead by Method D3559–90D, unless multiple in-furnace depositions are made. 14 If ultrasonic nebulization is used in the determination of arsenic by Methods 200.7, 200.8, or SM 3120 B, the arsenic must be in the pentavalent state to provide uniform signal response. 

For Methods 200.7 and 3120 B, both samples and standards must be diluted in the same mixed acid matrix concentration of nitric and hydrochloric acid with the addition of 100 μL of 30% hydrogen peroxide per 100 mL of solution. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain 1 mg/L of sodium hypochlorite. 15Starting January 23, 2006, analytical methods using the ICP–AES technology may not be used because the detection limits for these methods are 0.008 mg/L or higher. This restriction 

means that the two ICP–AES methods (EPA Method 200.7 and SM 3120 B) approved for use for the MCL of 0.05 mg/L may not be used for compliance determinations for the revised MCL 

of 0.010 mg/L. However, prior to January 23, 2006, systems may have compliance samples analyzed with these less sensitive methods. 16The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018. Or from the Hach Company, P.O. Box 

389, Loveland, CO 80539. 17The description for the Kelada-01 Method, ‘‘Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate,’’ Revision 1.2, August 2001, EPA # 821–B– 01–009 for cyanide is available from the National Technical Information Service (NTIS), PB 2001–108275, 5285 Port Royal Road, Springfield, VA 22161. The toll free telephone number is 800–553–6847. Note: A 450–W UV lamp may be used in this method instead of the 550–W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the 

method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met. 18The description for the QuikChem Method 10–204–00–1–X, ‘‘Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST and determination of cyanide by 

flow injection analysis,’’ Revision 2.1, November 30, 2000, for cyanide is available from Lachat Instruments, 6645 W. Mill Rd., Milwaukee, WI 53218. Telephone: 414–358–4200. 19 ‘‘Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,’’ Vol. 1, EPA 815–R–00–014, August 2000. Available at NTIS, PB2000–106981. 20 Method OIA–1677, DW ‘‘Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry,’’ January 2004. EPA–821–R–04–001, Available from ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842–9010. 21Sulfide levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide method to determine if a sulfide in- terference is present, and treat samples accordingly. 22Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last 

two digits in the method number. The methods listed are the only online versions that may be used. 23 Method D6508, Rev. 2, ‘‘Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,’’ available from Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: 508/482–2131, Fax: 508/482–3625. 

* * * * * 

■ 14. Section 141.24 is amended as 

follows: 

■ a. By revising the introductory text of 

paragraph (e)(1). 

■ b. By revising entries 23, 24, 26, 30, 

49, and 50 in the table to paragraph 

(e)(1). 

■ c. By adding a new footnote 5 to the 

table to paragraph (e)(1). 

§ 141.24 Organic chemicals, sampling and 

analytical requirements. 

* * * * * 

(e) * * * 

(1) The following documents are 

incorporated by reference. This 

incorporation by reference was 

approved by the Director of the Federal 

Register in accordance with 5 U.S.C. 

552(a) and 1 CFR Part 51. Copies may 

be inspected at EPA’s Drinking Water 

Docket, 1301 Constitution Avenue, NW., 

EPA West, Room 3334, Washington, DC 

20460 (Telephone: 202–566–2426); or at 

the National Archives and Records 

Administration (NARA). For 

information on the availability of this 

material at NARA, call 202–741–6030, 

or go to: http://www.archives.gov/ 

federal_register/ 

code_of_federal_regulations/ 

ibr_locations.html. Method 508A and 

515.1 are in Methods for the 

Determination of Organic Compounds 

in Drinking Water, EPA/600/4–88–039, 

December 1988, Revised, July 1991. 

Methods 547, 550 and 550.1 are in 

Methods for the Determination of 

Organic Compounds in Drinking 

Water—Supplement I, EPA/600–4–90–

020, July 1990. Methods 548.1, 549.1, 

552.1 and 555 are in Methods for the 

Determination of Organic Compounds 

in Drinking Water—Supplement II, 

EPA/600/R–92–129, August 1992. 

Methods 502.2, 504.1, 505, 506, 507, 

508, 508.1, 515.2, 524.2 525.2, 531.1, 

551.1 and 552.2 are in Methods for the 

Determination of Organic Compounds 

in Drinking Water––Supplement III, 

EPA/600/R–95–131, August 1995. 

Method 1613 is titled ‘‘Tetra–through 

Octa–Chlorinated Dioxins and Furans 

by Isotope–Dilution HRGC/HRMS,’’

EPA/821–B–94–005, October 1994. 

These documents are available from the 

National Technical Information Service, 

NTIS PB91–231480, PB91–146027, 

PB92–207703, PB95–261616 and PB95–

104774, U.S. Department of Commerce, 

5285 Port Royal Road, Springfield, 

Virginia 22161. The toll free number is: 

800–553–6847. Method 6651 shall be 

followed in accordance with Standard 

Methods for the Examination of Water 

and Wastewater, 18th edition (1992), 

19th edition (1995), or 20th edition 

(1998), American Public Health 

Association (APHA); any of these three 

editions may be used. Method 6610 

shall be followed in accordance with 

Standard Methods for the Examination 

of Water and Wastewater, (18th Edition 

Supplement) (1994), or with the 19th 

edition (1995) or 20th edition (1998) of 

Standard Methods for the Examination 

of Water and Wastewater; any of these 

publications may be used. The APHA 

documents are available from APHA, 

1015 Fifteenth Street NW., Washington, 

DC 20005. Other required analytical test 

procedures germane to the conduct of 

these analyses are contained in 

Technical Notes on Drinking Water 

Methods, EPA/600/R–94–173, October 

1994, NTIS PB95–104766. EPA Methods 

515.3 and 549.2 are available from U.S. 


rwilkins on PROD1PC63 with RULES
Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 11245 

Environmental Protection Agency, 

National Exposure Research Laboratory 

(NERL)–Cincinnati, 26 West Martin 

Luther King Drive, Cincinnati, OH 

45268. ASTM Method D 5317–93, 98 

(Reapproved 2003) is available in the 

Annual Book of ASTM Standards, 

(1999), Vol. 11.02, ASTM International, 

100 Barr Harbor Drive, West 

Conshohocken, PA 19428, any edition 

containing the cited version of the 

method may be used. EPA Method 

515.4, ‘‘Determination of Chlorinated 

Acids in Drinking Water by LiquidLiquid Microextraction, Derivatization 

and Fast Gas Chromatography with 

Electron Capture Detection,’’ Revision 

1.0, April 2000, EPA/815/B–00/001 and 

EPA Method 552.3, ‘‘Determination of 

Haloacetic Acids and Dalapon in 

Drinking Water by Liquid-Liquid 

Microextraction, Derivatization, and Gas 

Chromatography with Electron Capture 

Detection,’’ Revision 1.0, July 2003, EPA 

815–B–03–002, can be accessed and 

downloaded directly online at http:// 

www.epa.gov/safewater/methods/

sourcalt.html. Syngenta Method AG–

625, ‘‘Atrazine in Drinking Water by 

Immunoassay,’’ February 2001, is 

available from Syngenta Crop 

Protection, Inc., 410 Swing Road, P.O. 

Box 18300, Greensboro, NC 27419. 

Telephone: 336–632–6000. Method 

531.2 ‘‘Measurement of Nmethylcarbamoyloximes and Nmethylcarbamates in Water by Direct 

Aqueous Injection HPLC with 

Postcolumn Derivatization,’’ Revision 

1.0, September 2001, EPA 815–B–01–

002, can be accessed and downloaded 

directly online at http://www.epa.gov/

safewater/methods/sourcalt.html. 

Contaminant EPA Method1 Standard 

Methods ASTM Other 

* * * * * * * 

23. 2,4–D 4 (as acids, salts, and esters) ............................................ 515.2, 555, 

515.1, 515.3, 

515.4.

.................... D5317–93, 98 

(Reapproved 

2003).

24. 2,4,5–TP4 (Silvex) ........................................................................ 515.2, 555, 

515.1, 515.3, 

515.4.

.................... D5317–93, 98 

(Reapproved 

2003).

* * * * * * * 

26. Atrazine 2 ....................................................................................... 507, 525.2, 

508.1, 505, 

551.1.

.................... ............................ Syngenta 5 AG–625 

* * * * * * * 

30. Dalapon ........................................................................................ 552.1 515.1, 

552.2, 515.3, 

515.4, 552.3.

* * * * * * * 

49. Pentachlorophenol ........................................................................ 515.2, 525.2, 

555, 515.1, 

515.3, 515.4.

.................... D5317–93, 98 

(Reapproved 

2003).

50. Picloram 4 ...................................................................................... 515.2, 555, 

515.1, 515.3, 

515.4.

.................... D5317–93, 98 

(Reapproved 

2003).

* * * * * * * 

1For previously approved EPA methods which remain available for compliance monitoring until June 1, 2001, see paragraph (e)(2) of this section. 2Substitution of the detector specified in Method 505, 507, 508, or 508.1 for the purpose of achieving lower detection limits is allowed as follows: Either an electron capture or nitrogen phosphorus detector may be used provided all regulatory requirements and quality control criteria are 

met. 

* * * * * 

4Accurate determination of the chlorinated esters requires hydrolysis of the sample as described in EPA Methods 515.1, 515.2, 515.3, 515.4, 

and 555 and ASTM Method D 5317–93, 98 (Reapproved 2003). 5This method may not be used for the analysis of atrazine in any system where chlorine dioxide is used for drinking water treatment. In samples from all other systems, any result for atrazine generated by Method AG–625 that is greater than one-half the maximum contaminant level 

(MCL) (in other words, greater than 0.0015mg/L or 1.5 μg/L) must be confirmed using another approved method for this contaminant and should 

use additional volume of the original sample collected for compliance monitoring. In instances where a result from Method AG–625 triggers such 

confirmatory testing, the confirmatory result is to be used to determine compliance. 

* * * * * ■ 15. Section 141.25 is amended by 

revising the table in paragraph (a) to 

read as follows: 

§ 141.25 Analytical methods for 

radioactivity. 

(a) * * * 

Contaminant Methodology 

Reference (Method of Page Number) 

EPA1 EPA2 EPA3 EPA4 SM 5 ASTM 6 USGS7 DOE8 Other 

Naturally Occurring: 

Gross alpha 11 and beta ..... Evaporation ............ 900.0 p. 1 ... 00–01 p. 1 ........ 302, 7110 B, 

7110 B–00.

................ R–1120–76.

Gross alpha 11 ..................... Coprecipitation ....... ................ .......... 00–02 ............... 7110 C, 7110 

C–00.


rwilkins on PROD1PC63 with RULES
11246 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

Contaminant Methodology 

Reference (Method of Page Number) 

EPA1 EPA2 EPA3 EPA4 SM 5 ASTM 6 USGS7 DOE8 Other 

Radium 226 ........................ Radon emanation ... 903.1 p. 16 Ra–04 p. 19 ...... 305, 7500–Ra 

C, 7500–

Ra C–01.

D3454–97 R–1141–76 Ra-04 ..... NY9, 

Radiochemical ........ 903.0 p. 13 Ra-03 ............... 304, 7500–Ra 

B, 7500–Ra 

B–01.

D2460–97 R–1140–76 ................ GA14

Radium 228 ........................ Radiochemical ........ 904.0 p. 24 Ra-05 p. 19 ...... 7500–Ra D, 

7500–Ra 

D–01.

................ R–1142–76 ................ NY9, 

NJ 10, 

GA14

Uranium 12 ........................... Radiochemical ........ 908.0 .......... ............ ............... 7500–U B, 

7500–U B–

00.

Fluorometric ........... 908.1 .......... ............ ............... 7500–U C 

(17th Ed.).

D2907–97 R–1180–76, 

R–1181–

76.

U–04.

ICP–MS .................. 200.8 13 .......... ............ ............... 3125 ............. D5673–03.

Alpha Spectrometry ................ .......... 00–07 p. 33 ...... 7500–U C 

(18th, 19th, 

or 20th 

Ed.), 7500–

U C–00.

D3972–

97, 02.

R–1182–76 U–02.

Laser 

Phosphorimetry.

................ .......... ............ ............... ...................... D5174–

97, 02.

Man-Made: 

Radioactive Cesium ............ Radiochemical ........ 901.0 p. 4 ... ............ ............... 7500–Cs B, 

7500–Cs 

B–00.

D2459–72 R–1111–76.

Gamma Ray Spectrometry.901.1 .......... ............ p. 92 ...... 7120, 7120–

97.

D3649–

91, 98a.

R–1110–76 4.5.2.3.

Radioactive Iodine .............. Radiochemical ........ 902.0 p. 6 ... ............ ............... 7500–I B, 

7500–I B–

00.

p. 9 ... ............ ............... 7500–I C, 

7500–I C–

00.

7500–I D, 

7500–I D–

00.

D3649–

91, 98a.

Gamma Ray Spectrometry.901.1 .......... ............ p. 92 ...... 7120, 7120–

97.

D4785–

93, 00a.

.................... 4.5.2.3.

Radioactive Strontium 89, 

90.

Radiochemical ........ 905.0 p. 29 Sr–04 p. 65 ...... 303, 7500–Sr 

B, 7500–Sr 

B–01.

................ R–1160–76 Sr–01, 

Sr–02.

Tritium ................................. Liquid Scintillation .. 906.0 p. 34 H–02 .. p. 87 ...... 306, 7500– 3 H B, 

7500–3 H 

B–00.

D4107–

91, 98 

(Reapproved 

2002).

R–1171–76.

Gamma Emitters ................. Gamma Ray Spectrometry.901.1 .......... ............ p. 92 ...... 7120, 7120–

97.

D3649–

91, 98a.

R–1110–76 Ga–01–R.

902.0 .......... ............ ............... 7500–Cs B, 

7500–Cs 

B–00.

D4785–

93, 00a.

901.0 .......... ............ ............... 7500–I B, 

7500–I B–

00.

The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 and 13 through 14 was approved by the Director 

of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining 

these documents can be obtained from the Safe Drinking Water Hotline at 800–426–4791. Documents may be inspected at EPA’s Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., Room 3334 , Washington, DC 20460 (Telephone: 202–566–2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202–741–6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. 1 ‘‘Prescribed Procedures for the Measurement of Radioactivity in Drinking Water,’’ EPA 600/4–80–032, August 1980. Available at the U.S. Department of Commerce, National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161 (Telephone 800–553–6847), PB 80–224744. 2 ‘‘Interim Radiochemical Methodology for Drinking Water,’’ EPA 600/4–75–008 (revised), March 1976. Available NTIS, ibid. 3 ‘‘Radiochemistry Procedures Manual,’’ EPA 520/5–84–006, December 1987. Available NTIS, ibid. 4 ‘‘Radiochemical Analytical Procedures for Analysis of Environmental Samples,’’ March 1979. Available at NTIS, ibid. EMSL LV 053917. 5 ‘‘Standard Methods for the Examination of Water and Wastewater,’’ 13th, 17th, 18th, 19th or 20th edition, 1971, 1989, 1992, 1995, 1998. Available at American Public Health Association, 

1015 Fifteenth Street, NW., Washington, DC 20005. Methods 302, 303, 304, 305 and 306 are only in the 13th edition. Methods 7110B, 7500–Ra B, 7500–Ra C, 7500–Ra D, 7500–U B, 

7500–Cs B, 7500–I B, 7500–I C, 7500–I D, 7500–Sr B, and 7500–3H B are in the 17th, 18th, 19th and 20th editions. Method 7110 C is in the 18th, 19th and 20th editions. Method 7500–U 

C Fluorometric Uranium is only in the 17th Edition, and 7500–U C Alpha spectrometry is only in the 18th, 19th and 20th editions. Method 7120 is only in the 19th and 20th editions. Method 

3125 is only in the 20th edition. Methods 7110 B–00, 7110 C–00, 7500–Ra B–01, 7500–Ra C–01, 7500–Ra D–01, 7500–U B–00, 7500–U C–00, 7500–I B–00, 7500–I C–00, 7500–I D–00, 

7120–97, 7500–Sr B–01, and 7500–3H B–00 are available online at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is 

designated by the last two digits in the method number. The methods listed are the only online versions that may be used. 6Annual Book of ASTM Standards, Vol. 11.01 and 11.02, 2002; ASTM International; any year containing the cited version of the method may be used. Copies of these two volumes and 

the 2003 version of D 5673–03 may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428–2959. 7 ‘‘Methods for Determination of Radioactive Substances in Water and Fluvial Sediments,’’ Chapter A5 in Book 5 of Techniques of Water-Resources Investigations of the United States Geological Survey, 1977. Available at U.S. Geological Survey (USGS) Information Services, Box 25286, Federal Center, Denver, CO 80225–0425. 8 ‘‘EML Procedures Manual,’’ 28th (1997) or 27th (1990) Editions, Volumes 1 and 2; either edition may be used. In the 27th Edition Method Ra-04 is listed as Ra-05 and Method Ga-01–R is listed as Sect. 4.5.2.3. Available at the Environmental Measurements Laboratory, U.S. Department of Energy (DOE), 376 Hudson Street, New York, NY 10014–3621. 9 ‘‘Determination of Ra–226 and Ra–228 (Ra–02),’’ January 1980, Revised June 1982. Available at Radiological Sciences Institute for Laboratories and Research, New York State Department of Health, Empire State Plaza, Albany, NY 12201. 10 ‘‘Determination of Radium 228 in Drinking Water,’’ August 1980. Available at State of New Jersey, Department of Environmental Protection, Division of Environmental Quality, Bureau of 

Radiation and Inorganic Analytical Services, 9 Ewing Street, Trenton, NJ 08625. 11Natural uranium and thorium-230 are approved as gross alpha calibration standards for gross alpha with co-precipitation and evaporation methods; americium-241 is approved with coprecipitation methods. 12 If uranium (U) is determined by mass, a 0.67 pCi/μg of uranium conversion factor must be used. This conversion factor is based on the 1:1 activity ratio of U–234 and U–238 that is 

characteristic of naturally occurring uranium. 13 ‘‘Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma-Mass Spectrometry,’’ Revision 5.4, which is published in ‘‘Methods for the Determination of Metals in Environmental Samples—Supplement I,’’ ’ EPA 600–R–94–111, May 1994. Available at NTIS, PB 95–125472. 


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14 ‘‘The Determination of Radium-226 and Radium-228 in Drinking Water by Gamma-ray Spectrometry Using HPGE or Ge(Li) Detectors,’’ Revision 1.2, December 2004. Available from the 

Environmental Resources Center, Georgia Institute of Technology, 620 Cherry Street, Atlanta, GA 30332–0335, USA, Telephone: 404–894–3776. This method may be used to analyze for radium-226 and radium-228 in samples collected after January 1, 2005 to satisfy the radium-226 and radium-228 monitoring requirements specified at 40 CFR 141.26. 

* * * * * 

■ 16. Section 141.74 is amended as 

follows: 

■ a. By revising the entry for turbidity 

in the table in paragraph (a)(1). 

■ b. By revising footnotes 1, 8, 10, 11, 

and 12 to the table in paragraph (a)(1). 

■ c. By adding footnote 13 to the table 

in paragraph (a)(1). 

■ d. By revising paragraph (a)(2). 

§ 141.74 Analytical and monitoring 

requirements. 

(a) * * * 

(1) * * * 

Organism Methodology Citation 1

* * * * * * * 

Turbidity 13 ..................... Nephelometric Method ........................................................................................................................ 2130 B 

Nephelometric Method ........................................................................................................................ 180.1 9

Great Lakes Instruments ..................................................................................................................... Method 2 10

Hach FilterTrak .................................................................................................................................... 10133 12

* * * * * 

1Except where noted, all methods refer to Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition 

(1995), or 20th edition (1998), American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used. In addition, the following online versions may also be used: 2130 B–01, 9215 B–00, 9221 A, 

B, C, E–99, 9222 A, B, C, D–97, and 9223 B–97. Standard Methods Online are available at http://www.standardmethods.org. The year in which 

each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed 

are the only Online versions that may be used. 

* * * * * 

8A–1 broth may be held up to 7 days in a tightly closed screw cap tube at 4 °C. 9 ‘‘Methods for the Determination of Inorganic Substances in Environmental Samples,’’ EPA/600/R–93/100, August 1993. Available at NTIS, 

PB94–121811. 10GLI Method 2, ‘‘Turbidity,’’ November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, WI 53223. 11A description of the SimPlate method, ‘‘IDEXX SimPlate TM HPC Test Method for Heterotrophs in Water,’’ November 2000, can be obtained 

from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092, telephone (800) 321–0207. 12A description of the Hach FilterTrak Method 10133, ‘‘Determination of Turbidity by Laser Nephelometry,’’ January 2000, Revision 2.0, can be 

obtained from; Hach Co., P.O. Box 389, Loveland, CO 80539–0389, telephone: 800–227–4224. 13Styrene divinyl benzene beads (e.g. AMCO-AEPA–1 or equivalent) and stabilized formazin (e.g. Hach StablCal TM or equivalent) are acceptable substitutes for formazin. 

(2) Public water systems must 

measure residual disinfectant 

concentrations with one of the 

analytical methods in the following 

table. If approved by the State, residual 

disinfectant concentrations for free 

chlorine and combined chlorine also 

may be measured by using DPD 

colorimetric test kits. In addition States 

may approve the use of the ITS free 

chlorine test strip for the determination 

of free chlorine. Use of the test strips is 

described in Method D99–003, ‘‘Free 

Chlorine Species (HOCl- and OCl-) by 

Test Strip,’’ Revision 3.0, November 21, 

2003, available from Industrial Test 

Systems, Inc., 1875 Langston St., Rock 

Hill, SC 29730. Free and total chlorine 

residuals may be measured 

continuously by adapting a specified 

chlorine residual method for use with a 

continuous monitoring instrument 

provided the chemistry, accuracy, and 

precision remain the same. Instruments 

used for continuous monitoring must be 

calibrated with a grab sample 

measurement at least every five days, or 

with a protocol approved by the State. 

Residual Methodology SM 1 SM Online 2 Other 

Free Chlorine ............. Amperometric Titration ................................... 4500–Cl D .................. 4500–Cl D–00 ............ D1253–03 3

DPD Ferrous Titrimetric ................................. 4500–Cl F .................. 4500–Cl F–00.

DPD Colorimetric ........................................... 4500–Cl G .................. 4500–Cl G–00.

Syringaldazine (FACTS) ................................ 4500–Cl H .................. 4500–Cl H–00.

Total Chlorine ............. Amperometric Titration ................................... 4500–Cl D .................. 4500–Cl D–00 ............ D1253–03 3

Amperometric Titration (low level measurement).4500–Cl E .................. 4500–Cl E–00.

DPD Ferrous Titrimetric ................................. 4500–Cl F .................. 4500–Cl F–00.

DPD Colorimetric ........................................... 4500–Cl G .................. 4500–Cl G–00.

Iodometric Electrode ...................................... 4500–Cl I ................... 4500–Cl I–00.

Chlorine Dioxide ......... Amperometric Titration ................................... 4500–ClO2 C ............. 4500–ClO2 C–00.

DPD Method ................................................... 4500–ClO2 D.

Amperometric Titration ................................... 4500–ClO2 E .............. 4500–ClO2 E–00.

Spectrophotometric ........................................ .................................... .................................... 327.0, Revision 1.1 4

Ozone ......................... Indigo Method ................................................ 4500–O3 B ................. 4500–O3 B–97.

1All the listed methods are contained in the 18th, 19th, and 20th editions of Standard Methods for the Examination of Water and Wastewater, 

1992, 1995, and 1998; the cited methods published in any of these three editions may be used. 2Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard 

Methods Committee is designated by the last two digits in the method number. The methods listed are the only Online versions that may be 

used. 3Annual Book of ASTM Standards, Vol. 11.01, 2004 ; ASTM International; any year containing the cited version of the method may be used. 

Copies of this method may be obtained from ASTM International, 100 Barr Harbor Drive, P.O. Box C700 West Conshohocken, PA 19428–2959. 4EPA Method 327.0, Revision 1.1, ‘‘Determination of Chlorine Dioxide and Chlorite Ion in Drinking Water Using Lissamine Green B and Horseradish Peroxidase with Detection by Visible Spectrophotometry,’’ USEPA, May 2005, EPA 815–R–05–008. Available online at http:// 

www.epa.gov/safewater/methods/sourcalt.html. 


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11248 Federal Register / Vol. 72, No. 47 / Monday, March 12, 2007 / Rules and Regulations 

* * * * * 

PART 143—NATIONAL SECONDARY 

DRINKING WATER REGULATIONS 

■ 17. The authority citation for part 143 

continues to read as follows: 

Authority: 42 U.S.C. 300f et seq. 

■ 18. Section § 143.4 is amended by 

revising the table in paragraph (b) to 

read as follows: 

§ 143.4 Monitoring. 

* * * * * 

(b) * * * 

Contaminant EPA ASTM 3 SM 4 18th and 19th ed. SM 4 20th ed. SM 7 Online Other 

1. Aluminum ...................... 200.7 2 ......................... 3120 B .............................. 3120 B .............................. 3120 B–99.

200.8 2 ......................... 3113 B .............................. .......................................... 3113 B–99.

200.9 2 ......................... 3111 D ............................. .......................................... 3111 D–99.

2. Chloride ........................ 300.0 1, 

300.1 6

D4327–97, 03 4110 B .............................. 4110 B .............................. 4110 B–00.

4500–Cl– D ....................... 4500–Cl– D ....................... 4500–Cl– D–97.

D512–89 (Reapproved 

1999) B.

4500–Cl– B ....................... 4500–Cl– B ....................... 4500–Cl– B–97.

D6508, Rev. 2 8

3. Color ............................. ................ ......................... 2120 B .............................. 2120 B .............................. 2120 B–01.

4. Foaming Agents ........... ................ ......................... 5540 C ............................. 5540 C ............................. 5540 C–00.

5. Iron ............................... 200.7 2 ......................... 3120 B .............................. 3120 B .............................. 3120 B–99.

200.9 2 ......................... 3111 B .............................. .......................................... 3111 B–99.

......................... 3113 B .............................. .......................................... 3113 B–99.

6. Manganese ................... 200.7 2 ......................... 3120 B .............................. 3120 B .............................. 3120 B–99.

200.8 2 ......................... 3111 B .............................. .......................................... 3111 B–99.

200.9 2 ......................... 3113 B .............................. .......................................... 3113 B–99.

7. Odor .............................. ......................... 2150 B .............................. 2150 B .............................. 2150 B–97.

8. Silver ............................. 200.7 2 ......................... 3120 B .............................. 3120 B .............................. 3120 B–99. I–3720–85 5

200.8 2 ......................... 3111 B .............................. .......................................... 3111 B–99.

200.9 2 ......................... 3113 B .............................. .......................................... 3113 B–99.

9. Sulfate .......................... 300.0 1, 

300.1 6

D4327–97, 03 4110 B .............................. 4110 B .............................. 4110 B–00.

375.2 1 ......................... 4500–SO4 2– F ................. 4500–SO4 2– F.

4500–SO4 2– C, D ............ 4500–SO4 2– C, D.

D516–90, 02 ... 4500–SO4 2– E ................. 4500–SO4 2– E.

D6508, Rev. 2 8

10. Total Dissolved Solids ......................... 2540 C ............................. 2540 C ............................. 2540 C–97.

11. Zinc ............................. 200.7 2 ......................... 3120 B .............................. 3120 B .............................. 3120 B–99.

200.8 2 ......................... 3111 B .............................. .......................................... 3111 B–99.

The procedures shall be done in accordance with the documents listed below. The incorporation by reference of the following documents was approved by the Director of the Federal Register in accordance with 5 U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these documents can 

be obtained from the Safe Drinking Water Hotline at 800–426–4791. Documents may be inspected at EPA’s Drinking Water Docket, EPA West, 1301 Constitution Avenue, NW., Room 3334, 

Washington, DC (Telephone: 202–566–2426); or at the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202–741–6030, 

or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. 1 ‘‘Methods for the Determination of Inorganic Substances in Environmental Samples,’’ EPA/600/R–93–100, August 1993. Available at NTIS, PB94–120821. 2 ‘‘Methods for the Determination of Metals in Environmental Samples—Supplement I,’’ EPA/600/R–94–111, May 1994. Available at NTIS, PB 95–125472. 3Annual Book of ASTM Standards, 1994, 1996, 1999, or 2004, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. Copies may 

be obtained from the ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428. 4Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), or 20th edition (1998). American Public Health Association, 1015 Fifteenth 

Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except that the versions of 3111 B, 3111 D, and 3113 B in the 20th edition 

may not be used. 5 Method I–3720–85, Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A–1, 3rd ed., 1989. Available from Information Services, U.S. Geological 

Survey, Federal Center, Box 25286, Denver, CO 80225–0425. 6 ‘‘Methods for the Determination of Organic and Inorganic Compounds in Drinking Water,’’ Vol. 1, EPA 815-R–00–014, August 2000. Available at NTIS, PB2000–106981. 7Standard Methods Online are available at http://www.standardmethods.org. The year in which each method was approved by the Standard Methods Committee is designated by the last 

two digits in the method number. The methods listed are the only online versions that may be used. 8 Method D6508, Rev. 2, ‘‘Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte,’’ available from Waters Corp, 34 Maple St., Milford, MA, 01757, Telephone: 508/482–2131, Fax: 508/482–3625. 

PART 430—THE PULP, PAPER, AND 

PAPERBOARD POINT SOURCE 

CATEGORY 

■ 19. The authority citation for part 430 

continues to read as follows: 

Authority: Sections 301, 304, 306, 307, 

308, 402, and 501 of the Clean Water Act, as 

amended, (33 U.S.C. 1311, 1314, 1316, 1317, 

1318, 1342, and 1361), and Section 112 of the 

Clean Air Act, as amended (42 U.S.C. 7412). 

■ 20. Section 430.02 is amended by 

adding paragraph (g) to read as follows: 

§ 430.02 Monitoring requirements. 

* * * * * 

(g) Analyst may use NCASI Method 

CP–86.07, ‘‘Chlorinated Phenolics in 

Water by In situ Acetylation and GC/MS 

Determination’’ (January 2002) for 

determination of certain chlorinated 

phenols, chlorinated guaiacols, 

chlorinated catechols, chlorinated 

benzaldehydes (i.e., vanillins and 

syringaldehydes), and trichlorsyringol 

(analytes specified in the method) in 

bleach plant filtrate as an alternative to 

EPA Method 1653. NCASI Method CP–

86.07 is available from the Publications 

Coordinator, NCASI, P.O. Box 13318, 

Research Triangle Park, NC 27709–3318. 

Telephone: 919–588–1987. 

PART 455—PESTICIDE CHEMICALS 

■ 21. The authority citation for Part 455 

continues to read as follows: 

Authority: Secs. 301, 304, 306, 307, and 

501, Pub. L. 92–500, 86 Stat. 816, Pub. L. 95–

217, 91 Stat. 156, and Pub. L. 100–4 (33 

U.S.C. 1311, 1314, 1316, 1317, 1361). 

■ 22. Section 455.50 is revised to read 

as follows: 

§ 455.50 Identification of test procedures. 

The pesticide active ingredients to 

which this section applies and for 

which effluent limitations guidelines 

and standards are specified in this Part 

are named, together with the Chemical 

Abstracts Service (CAS) number 

(provided to assist in identifying the 

pesticide active ingredient only) and 

analytical method(s) designation(s) in 

Table IG at 40 CFR 136.3(a). Except as 

provided in 40 CFR 136.5, the discharge 

parameter values required under the 

Clean Water Act must be determined by 

one of the analytical methods cited and 

described in Table IG at 40 CFR 

136.3(a). Pesticide manufacturers may 

not use the analytical method cited in 


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Table IB, Table IC, or Table ID of 40 CFR 

136.3(a) to make these determinations 

(except where the method cited in those 

tables is identical to the method 

specified in Table IG at 40 CFR 

136.3(a)). The full texts of the analytical 

methods cited in Table IG at 40 CFR 

136.3(a) are contained in the Methods 

For The Determination of 

Nonconventional Pesticides In 

Municipal and Industrial Wastewater, 

Volume I, EPA 821-R–93–010A (August 

1993 Revision I) and Volume II, EPA 

821-R–93–010B (August 1993) (the 

‘‘Compendium’’). Each pesticide 

chemical manufacturer that is required 

to determine discharge parameter values 

under this Part using one of the 

analytical methods cited in Table IG at 

40 CFR 136.3(a) must request in writing 

a copy of the Compendium from the 

permit authority or local control 

authority (as applicable) prior to 

determining such discharge parameter 

values, unless the manufacturer already 

has a copy. 

■ 23. Part 455 is amended by removing 

and reserving Table 7 to Part 455. 

PART 465—COIL COATING POINT 

SOURCE CATEGORY 

■ 24. The authority citation for Part 465 

continues to read as follows: 

Authority: Secs. 301,304 (b), (c), (e), and 

(g), 306 (b) and (c), 307 (b) and (c), and 501 

of the Clean Water Act (the Federal Water 

Pollution Control Act of 1972, as amended by 

the Clean Water Act of 1977)(the ‘‘Act’’); 33 

U.S.C. 1311, 1314 (b), (c), (e), and (g), 1316 

(b) and (c), 1317 (b) and (c), and 1361; 86 

Stat. 816, Pub. L. 92–500; 91 Stat. 1567, Pub. 

L. 95–217. 

■ 25. Section 465.03 is amended by 

revising paragraph (c) to read as follows: 

§ 465.03 Monitoring and reporting 

requirements. 

* * * * * 

(c) The analytical method required for 

determination of petroleum 

hydrocarbons (non-polar material) is 

given under the listing for ‘‘oil and 

grease’’ at 40 CFR 136.3(a), Table IB and 

must be used after December 31, 2005. 

* * * * * 

[FR Doc. 07–1073 Filed 3–9–07; 8:45 am] 

BILLING CODE 6560–50–P 


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