# Clean Water Act Methods Update Rule for the Analysis of Effluent

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URL: https://www.frixlaw.com/law-library/documents/fr%3A2015-02841

## Record

- **Collection:** Federal Register
- **Document type:** Proposed Rule
- **Published:** February 19, 2015
- **Citation:** 80 FR 8956

## Text

ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 136
[EPA-HQ-OW-2014-0797; FRL-9920-55-OW]
RIN 2040-AF48
Clean Water Act Methods Update Rule for the Analysis of Effluent

AGENCY:

Environmental Protection Agency (EPA).

ACTION:

Proposed rule.

SUMMARY:

EPA proposes changes to pollutant analysis methods that are used by industries and municipalities to analyze the chemical, physical, and biological components of wastewater and other environmental samples that are required by regulations under the Clean Water Act. EPA designed the proposed changes to increase flexibility for the regulated community, improve data quality, and update CWA methods to keep current with technology advances and analytical methods science. EPA updates and revises the CWA analytical methods from time to time, the most recent updates being completed in 2012. The new set of proposed changes described in this notice include revisions to current EPA methods and new and/or revised methods published by voluntary consensus standard bodies, such as ASTM International and the Standard Methods Committee. EPA also proposes to approve certain methods reviewed under the alternate test procedures program and clarify the procedures for EPA approval of nationwide and limited use alternate test procedures. Further, EPA proposes amendments to the procedure for determination of the method detection limit to address laboratory contamination and to better account for intra-laboratory variability.

DATES:

Comments on this proposed rule must be received on or before April 20, 2015.

ADDRESSES:

Submit your comments, identified by Docket ID No. EPA-HQ-OW-2014-0797, by one of the following methods:

•
www.regulations.gov:
Follow the on-line instructions for submitting comments.

•
Email: OW-Docket@epa.gov,
Attention Docket ID number EPA-HQ-OW-2014-0797.

•
Mail:
Water Docket, Environmental Protection Agency, Mail code: 4203M, 1200 Pennsylvania Ave. NW., Washington, DC 20460. Attention Docket ID number EPA-HQ-OW-2014-0797. Please include a total of 3 copies.

•
Hand Delivery:
Water Docket, EPA Docket Center, EPA West Building, Room 3334, 1301 Constitution Ave. NW., Washington, DC, Attention Docket ID number EPA-HQ-OW-2014-0797. Such deliveries are only accepted during the Docket's normal hours of operation, and special arrangements should be made for deliveries of boxed information by calling 202-566-2426.

Instructions:
Direct your comments to Docket ID number EPA-HQ-OW-2014-0797. EPA's policy is that all comments received will be included in the public docket without change and may be made available online at
www.regulations.gov,
including any personal information provided, unless the comment includes information claimed to be Confidential Business Information (CBI) or other information whose disclosure is restricted by statute. Do not submit information that you consider to be CBI or otherwise protected through
www.regulations.gov
or email. The
www.regulations.gov
Web site is an “anonymous access” system, which means EPA will not know your identity or contact information unless you provide it in the body of your comment. If you send an email comment directly to EPA without going through
www.regulations.gov
your email address will be automatically captured and included as part of the comment that is placed in the public docket and made available on the Internet. If you submit an electronic comment, EPA recommends that you include your name and other contact information in the body of your comment and with any disk or CD-ROM you submit. If EPA cannot read your comment due to technical difficulties and cannot contact you for clarification, EPA may not be able to consider your comment. Electronic files should avoid the use of special characters, any form of encryption, and be free of any defects or viruses.

Docket:
All documents in the docket are listed in the
www.regulations.gov
index. Although listed in the index, some information in the docket is not publicly available,
e.g.,
CBI or other information whose disclosure is restricted by statute. Certain other material, such as copyrighted material, will be publicly available only in hard copy. Publicly available docket materials are available either electronically in
www.regulations.gov
or in hard copy at the Water Docket in EPA Docket Center, EPA/DC, EPA West William J. Clinton Building, Room 3334, 1301 Constitution Ave. NW., Washington, DC. The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. The telephone number for the Public Reading Room is 202-566-1744 and the telephone number for the Water Docket is 202-566-2426.

FOR FURTHER INFORMATION CONTACT:

Adrian Hanley, Engineering and Analysis Division (4303T), Office of Water, Environmental Protection Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460-0001; telephone: 202-564-1564; email:
hanley.adrian@epa.gov.

SUPPLEMENTARY INFORMATION:

Table of Contents

I. General Information

II. Overview

III. Statutory Authority

IV. Purpose and Summary of Proposed Rule

V. Statutory and Executive Order Reviews

I. General Information

A. Does this Action apply to me?

Entities potentially affected by the requirements of this proposed action include:

Category
Examples of potentially affected entities

State, Territorial, and Indian Tribal Governments
States, territories, and tribes authorized to administer the National Pollutant Discharge Elimination System (NPDES) permitting program; states, territories, and tribes providing certification under CWA section 401; state, territorial, and tribal owned facilities that must conduct monitoring to comply with NPDES permits.

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

Municipalities
Publicly Owned Treatment Works (POTWs) or other municipality owned facilities that must conduct monitoring to comply with NPDES permits.

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

B. What should I consider as I prepare my comments for EPA?

1. Submitting CBI.
Do not submit CBI to EPA through
www.regulations.gov
or email. Clearly mark the part or all of the information that you claim to be CBI. For CBI information in a disk that you mail to EPA, mark the outside of the disk as CBI and then identify electronically within the disk the specific information that is claimed as CBI. In addition to one complete version of the comment that includes information claimed as CBI, a copy of the comment that does not contain the information claimed as CBI must be submitted for inclusion in the public docket. Information so marked will not be disclosed except in accordance with procedures for handling and protection of CBI set forth in 40 CFR part 2.

2. Tips for Preparing Your Comments.
When submitting comments, remember to:

• Identify the rulemaking by Docket ID number and other identifying information (subject heading,
Federal Register
date and page number).

• Explain why you agree or disagree, suggest alternatives, and substitute language for your requested changes.

• Describe any assumptions and provide any technical information and/or data that you used.

• If you estimate potential costs or burdens, explain how you arrived at your estimate in sufficient detail to allow for it to be reproduced.

• Provide specific examples to illustrate your concerns, and suggest alternatives.

• Explain your views as clearly as possible, avoiding the use of profanity or personal threats.

• Make sure to submit your comments by the comment period deadline identified.

II. Overview

This preamble describes the reasons for the proposed rule; the legal authority for the proposed rule; a summary of the proposed changes and clarifications; and explanation of the abbreviations and acronyms used in this document. In addition, this preamble solicits comment and data from the public.

Abbreviations and Acronyms Used in the Preamble and Proposed Rule Text

AA: Atomic Absorption

ADMI: American Dye Manufacturers Institute

ASTM: ASTM International

ATP: Alternate Test Procedure

CAS: Chemical Abstract Services

CFR: Code of Federal Regulations

CWA: Clean Water Act

EPA: Environmental Protection Agency

FLAA: Flame Atomic Absorption Spectroscopy

GC: Gas Chromatograph

ICP/AES: Inductively Coupled Plasma—Atomic Emission Spectroscopy

ICP/MS: Inductively Coupled Plasma—Mass Spectrometry

LCS: Laboratory Control Sample

MS: Mass Spectrometry

MS/MSD: Matrix Spike/Matrix Spike Duplicate

NPDES: National Pollutant Discharge Elimination System

POTW: Publicly Owned Treatment Works

QA: Quality Assurance

QC: Quality Control

SM: Standard Methods

STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption Spectroscopy

USGS: United States Geological Survey

VCSB: Voluntary Consensus Standards Body

III. Statutory Authority

EPA proposes this regulation under the authorities of sections 301(a), 304(h), and 501(a) of the CWA, 33 U.S.C. 1311(a), 1314(h), and 1361(a). Section 301(a) of the CWA prohibits the discharge of any pollutant into navigable waters unless the discharge complies with, among other provisions, a NPDES permit issued under section 402 of the CWA. Section 304(h) of the CWA requires the Administrator of the EPA to “. . . promulgate guidelines establishing test procedures for the analysis of pollutants that shall include the factors which must be provided in any certification pursuant to [section 401 of the CWA] or permit application pursuant to [section 402 of the CWA].” Section 501(a) of the CWA authorizes the Administrator to “. . . prescribe such regulations as are necessary to carry out this function under [the CWA].” 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).

IV. Purpose and Summary of Proposed Rule

The CWA requires EPA to promulgate test procedures (analytical methods) for analyses required in NPDES permit applications and for reports required under NPDES permits. EPA codifies these approved test procedures at 40 CFR part 136. EPA regions, as well as authorized states, territories and tribes issue NPDES permits. These permits must include conditions designed to ensure compliance with the technology-based and water quality-based requirements of the CWA, including in many cases, restrictions on the quantity of specific pollutants that can be discharged as well as pollutant measurement and reporting requirements. Often, entities have a choice in deciding which approved test procedure they will use for a specific pollutant because EPA has approved the use of more than one.
1

1
NPDES permit regulations also specify that the approved method needs to be sufficiently sensitive. See 40 CFR 122.21.e.3.

The procedures for the analysis of pollutants required by CWA section 304(h) are a central element of the NPDES permit program. Examples of where these EPA analytical methods must be used include, among others, the following: (1) Applications for NPDES permits, (2) sampling or other reports required under NPDES permits, (3) other requests for quantitative or qualitative effluent data under the NPDES regulations, (4) State CWA 401 certifications and (5) sampling and analysis required under EPA's General Pre-Treatment Regulations for Existing and New Sources of Pollution 40 CFR 136.1 and 40 CFR 403.12(b)(5)(v).

Periodically, EPA proposes to update the approved methods in 40 CFR part 136. In general, the changes in this proposed action fall into the following categories: new and revised EPA methods and new and revised methods adopted by VCSBs; methods EPA has reviewed under EPA's national alternate test procedures (ATP) program and preliminarily concluded are appropriate for nationwide use; certain corrections to 40 CFR part 136; and amendments to the procedure for determination of the MDL primarily to address laboratory contamination and to better account for intra-laboratory variability. Collectively, EPA's current understanding indicates that adoption of these proposed revisions would improve data quality, update methods to keep current with technology advances, provide additional

clarity for ATPs, and provide the regulated community with greater flexibility.

The following paragraphs provide details on the proposed revisions.

A. Changes to 40 CFR 136.3 and Appendix A to Include New Versions of Previously Approved EPA Methods

EPA proposes revisions to the approved EPA Methods 608, 624, and 625 which it adopted in 1984, and proposes to make a minor correction to the parameter list in EPA Method 611. These four EPA methods are listed in Table IC at 40 CFR part 136. Methods 608 and 625 also are listed in Tables ID and IG, and Methods 624 and 625 are listed in Table IF. EPA also proposes minor corrections to microbiological methods 1600, 1603, 1680, and 1682. These four EPA methods are listed in Table IA at 40 CFR part 136, and Methods 1600 and 1603 are listed in Table IH.

1. Methods 608, 624, and 625

The proposed revisions take advantage of improvements in analytical technology and allow greater flexibility in order to accommodate future improvements to the methods and generally obviate any need for additional revisions. EPA revised these methods in collaboration with other EPA offices, states, and environmental laboratory organizations. The revisions conform to the following principles:

Updated Technology: EPA changed the GC columns from packed columns to capillary (open tubular) columns. Capillary columns provide greater resolution and decreased adsorption (loss) of the analytes and, therefore, result in a significant improvement in the accuracy (recovery) and precision of the results.

Method Flexibility: The revised methods allow greater method flexibility so that the methods more closely align with 40 CFR 136.6. This flexibility would make it easier for laboratories to make in-house improvements and technology updates in the future that will not compromise the original quality control acceptance criteria of the methods. Consistent with 40 CFR 136.6, EPA built into the methods procedures that will allow a laboratory to make limited changes to a method without applying for an ATP; however, the laboratory must document that the revisions produce results consistent with the QC acceptance criteria in the method in order to take advantage of the built-in flexibility. For example, the revised methods allow access to a greater list of compounds than the list of compounds determined by the original versions of these methods, provided that the laboratory can demonstrate acceptable accuracy and precision with these analytes in the specified matrices. The expanded list of compounds is an amalgamation of lists from Methods 1624, 1625, 1699 and other EPA methods that demonstrate the technology can be used to quantify these additional analytes. The revisions also allow more flexibility to adopt different extraction procedures, such as solid phase extraction. The revised methods include requirements for a laboratory to develop its own in-house QC acceptance criteria for tests of the laboratory control sample and tests of matrix spike and matrix spike duplicate samples, provided the LCS and MS/MSD meet minimum criteria specified in the method. The revisions also clarify that hydrogen can be used as a carrier gas for the methods. Some of the flexibility EPA proposes to add to the methods is currently specified in 40 CFR 136.6(b)(4)(xvi). Because EPA proposes to incorporate that flexibility directly into the method, EPA proposes to delete the corresponding text from 40 CFR 136.6.

Method Harmonization: EPA updated these methods to make them more consistent with the most recent updates of similar methods from the Office of Ground Water and Drinking Water and the Office of Resource Conservation and Recovery. EPA revised the required QC frequencies and standards (internal standards and surrogates) to more closely match the methods from other EPA analytical method programs. Laboratories that run methods from multiple EPA programs will benefit from these revisions.

2. Method 611

EPA proposes a minor correction to a parameter name in the parameter list of of EPA Method 611 (“Haloethers”). As currently listed, the compound with the CAS Registry Number 108-60-1 is bis(2-chloroisopropyl)ether. EPA proposes to correct the analyte name to 2,2′-oxybis(1-chloropropane), which matches the CAS Number 108-60-1. The original analyte name bis(2-chloroisopropyl)ether has a CAS number of 39638-32-9. EPA is unaware that this chemical has ever been in industrial production, and is therefore unlikely to be a compound of monitoring concern. Furthermore, it is not possible to procure an analytical standard reference material for the compound with CAS number 39638-32-9. The compound in the parameter list should be 2,2′-oxybis(1-chloropropane), CAS number 108-60-1.

3. Methods 1600, 1603, 1680, and 1682

EPA proposes the following changes for EPA microbiological methods 1600, 1603, 1680, and 1682. These changes correct typographical or other errors that EPA identified in the methods after publication. EPA proposes to revise all of these methods with new EPA document numbers and dates.

a. EPA Method 1600 for Enterococci using membrane filtration: In Table 3 Verification controls, EPA changed the negative control for brain heart infusion broth incubated at 45 °C from
E. coli
to
Enterobacter aerogenes. E. coli
is thermotolerant and
E. aerogenes
is not, so
E. coli
is not an appropriate negative control when heated.

b. EPA Method 1603 for
E. coli
using membrane filtration: In Section 11.5, EPA changed the number of colonies on a countable plate from 20-60 to 20-80 colonies. Sixty colonies was a typographical error. In addition the following sentence was inadvertently omitted and EPA included it: Sample volumes of 1-100 mL are normally tested at half-log intervals (
e.g.,
100, 30, 10, and 3 mL).

c. EPA Method 1680 for fecal coliforms using multiple tube fermentation: in Section 3.1 Definitions, the sentence “The predominant fecal coliform is
E. coli.”
should read “The predominant fecal coliform can be
E. coli.”

d. EPA Method 1682 for
Salmonella
by MSRV medium: (1) In Section 9.3, Table 2, the lab-prepared spike acceptance criteria should read “Detect—254%” and “Detect—287%” and (2) in Section 14.5, Table 9, the spiked
Salmonella
for Example 2, Liquid should read “3.7x10
8
CFU/mL.”

B. Methods Incorporated by Reference

Currently, hundreds of methods and ATPs are incorporated by reference within 40 CFR part 136. In most cases, 40 CFR part 136 contains multiple approved methods for a single pollutant and regulated entities often have a choice in the selected method. The proposed rule contains revisions to methods that will be incorporated by reference from two VCSBs: Standard Methods and ASTM. EPA proposed VCSB methods in compliance with the National Technology Transfer Act (see Section V.I below). The proposed VCSB methods are available on their respective VCSB Web sites to everyone at a cost determined by the VCSB, generally from $40 to $80. Both organizations also offer memberships or subscriptions that allow unlimited access to their methods. The cost of obtaining these methods is not a

significant financial burden for a discharger or environmental laboratory, making the methods reasonably available. The proposal also includes USGS methods and vendor ATPs that are incorporated by reference. The ATPs and USGS methods are available free of charge on the Web site for that organization. Therefore, EPA concludes that the proposed methods and ATPs incorporated by reference are reasonably available. The individual standards are discussed in greater detail below.

C. Changes to 40 CFR 136.3 to Include New Versions of Approved Standard Methods

EPA proposes to approve new versions of currently approved Standard Methods. The new versions of currently approved Standard Methods clarify or improve the instructions in the method, improve the QC instructions, or make editorial corrections. Consistent with the previous method update rule (77 FR 29767-29768), EPA proposes to generally approve and include in 40 CFR part 136 only the most recent version of a method published by the Standard Methods Committee by listing only one version of the method with the year of publication designated by the last four digits in the method number (
e.g.,
SM 3111 B-2011). The date indicates the latest revision date of the method. This allows use of a specific method in any edition that includes a method with the same method number and year of publication.

Most of the revisions that EPA proposes to Standard Methods previously approved in 40 CFR part 136 do not contain any substantive changes. The following describes the proposed non-substantive changes related to Standard Methods in 40 CFR part 136. Each entry contains the proposed Standard Methods number and date, the parameter, and a brief description of the analytical technique. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear.

The following changes would apply to Table IA at 40 CFR part 136:

1. SM 9221 (B,C,E,F)-2006, Coliform (fecal), Coliform (fecal) in presence of chlorine, Coliform (total), Coliform (total) in presence of chlorine,
E. coli,
most probable number (MPN), 5 tube 3 dilution.

2. SM 9223-2004,
E. coli,
multiple tube/multiple well.

3. SM 9230 (B,C)-2007, Fecal Streptococci, Enterococci, most probable number (MPN), 5 tube 3 dilution or membrane filtration.

The following changes would apply to Table IB at 40 CFR part 136:

1. SM 2120 B-2011, color, platinum cobalt method.

2. SM 2130 B-2011, turbidity, nephelometric method.

3. SM 2310 B-2011, acidity, titration using electrometric endpoint or phenolphthalein endpoint.

4. SM 2320 B-2011, alkalinity, electrometric or colorimetric titration to pH 4.5.

5. SM 2340 B-2011 and SM 2340 C-2011, hardness, by the calculation method or EDTA titration.

6. SM 2510 B-2011, conductivity, Wheatstone bridge method.

7. SM 2540 B-2011, SM 2540 C-2011, SM 2540 D-2011, SM 2540 E-2011, and SM 2540 F-2011, total, filterable, non-filterable, volatile, and settleable residue (solids, listed in the same order as the method numbers), all by gravimetric methodologies.

8. SM 2550 B-2010, temperature, thermometric.

9. SM 3111 B-2011, SM 3111 C-2011, SM 3111 D-2011, and SM 3111 E-2011, metals, direct aspiration AA methods with different gas mixtures. Each method has a different list of metals; no changes are proposed to these lists.

10. SM 3112 B-2011, metals, applicable to mercury, cold-vapor atomic absorption spectrometric method.

11. SM 3114 B-2011 and SM 3114 C-2011, total arsenic and total selenium, hydride generation/atomic absorption spectrometric methods. Both analyze total arsenic and total selenium.

12. SM 3120 B-2011, metals, ICP method; no changes are proposed for the approved list of metals.

13. SM 3125 B-2011, metals, ICP/MS method; no changes are proposed for the approved list of metals.

14. SM 3500-Al B-2011, aluminum, colorimetric method.

15. SM 3500-As B-2011, arsenic, colorimetric method (SDDC).

16. SM 3500-Ca B-2011, calcium, titrimetric method (EDTA).

17. SM 3500-Cr B-2011 and SM 3500-Cr C-2011, chromium, the “B” method uses a colorimetric method (diphenyl-carbazide) and is approved for total or dissolved chromium, the “C” method uses ion chromatography and is only approved for dissolved chromium.

18. SM 3500-Cu B-2011 and SM 3500-Cu C-2011, copper, both method sections use colorimetric methods, the “B” method uses a neocuproine reagent and the “C” method uses a bathocuproine reagent.

19. SM 3500-Fe B-2011, iron, colorimetric method (phenanthroline).

20. SM 3500-K B-2011 and SM 3500-K C-2011, potassium, the “B” method is a flame photometric method and the “C” method is an electrode method.

21. SM 3500-Mn B-2011, manganese, colorimetric method (persulfate).

22. SM 3500-Na B-2011, sodium, flame photometric method.

23. SM 3500-Pb B-2011, lead, colorimetric method (dithizone).

24. SM 3500-V B-2011, vanadium, colorimetric method (gallic acid).

25. SM 3500-Zn B-2011, zinc, colorimetric method (zincon).

26. SM 4110 (B-D)-2011, anions, ion chromatography; no changes are proposed for the approved analyte list.

27. SM 4140 B-2011, inorganic anions, capillary ion electrophoresis with indirect UV detection: No changes are proposed for the approved analyte list.

28. SM 4500-B B-2011, boron, spectrophotometer or filter photometer (curcumin).

29. SM 4500-Cl
−
(B-E)-2011, chloride, titrimetric: (silver nitrate), (mercuric nitrate), automated (ferricyanide), potentiometric titration

30. SM 4500-Cl (B-G)-2011, chlorine (residual), amperometric direct, amperometric direct (low level), iodometric direct, back titration ether end-point, titrimetric: N,N-diethyl-p-phenylenediamine with ferrous ammonium sulfate (DPD-FAS), spectrophotometric (DPD).

31. SM 4500-CN
−
(B-G)-2011, cyanide, manual distillation with MgCl
2
followed by: Titrimetric, spectrophotometric, manual, ion selective electrode, cyanide amenable to chlorination (CATC); manual distillation with MgCl
2
, followed by: Titrimetric or spectrophotometric.

32. SM 4500-F
−
(B-E)-2011, fluoride, manual distillation, followed by any of the following: Electrode, manual, colorimetric, fluoride dye reagent (SPADNS is the common name for the fluoride dye reagent which is a mixture of chemicals), automated complexone.

33. SM 4500-H
+
B-2011, hydrogen ion (pH), electrometric measurement.

34. SM 4500-NH
3
(B-H)-2011, ammonia (as nitrogen), manual distillation or gas diffusion (pH > 11), followed by any of the following: Titration, electrode, manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods; automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods.

35. SM 4500-NO
2
−
B-2011, nitrite (as nitrogen), spectrophotometric: Manual.

36. SM 4500-NO
3
−
D-2011, nitrate (as nitrogen), ion selective electrode.

37. SM 4500-NO
3
−
(E,F, H)-2011, nitrate-nitrite (as nitrogen), colorimetric: Cadmium reduction-manual and automated, and colorimetric: Automated hydrazine.

38. SM 4500-NO
3
−
(E,F)-2011, nitrite (as nitrogen), colorimetric: Cadmium reduction-manual and automated.

39. SM 4500-N
org
(B-D)-2011, total Kjeldahl nitrogen (as nitrogen, organic), semi-automated block digester colorimetric (distillation not required).

40. SM 4500-O (B-G), oxygen (dissolved), Winkler (azide modification), electrode.

41. SM 4500-P (B (5), E-H)-2011, phosphorus and ortho-phosphate, persulfate digestion, digestion, followed by any of the following: Manual or automated ascorbic acid reduction. The “B Part 5” method is the persulfate digestion procedure and is required prior to measurement of total phosphorus using SM 4500 P (E-H). The “E” through “G” methods are approved for both total phosphorus and ortho-phosphate. The “H” method is only approved for total phosphorous.

42. SM 4500-S
2−
(B-D, F,G)-2011, sulfide, sample pretreatment, titrimetric (iodine) analysis, colorimetric (methylene blue), ion selective electrode.

43. SM 4500-SiO
2
(C,E,F)-2011, silica, 0.45-micron filtration followed by any of the following: Colorimetric, manual or automated (Molybdosilicate).

44. SM 4500-SO
3
2−
B-2011, sulfite, titrimetric (iodine-iodate).

45. SM 4500-SO
4
2−
(C-G)-2011, sulfate, automated colorimetric, gravimetric, and turbidimetric.

46. SM 5210 B-2011, biochemical oxygen demand (BOD5), dissolved oxygen depletion.

47. SM 5220 (B-D)-2011, chemical oxygen demand (COD), titrimetric; spectrophotometric, manual or automatic.

48. SM 5310 (B-D)-2011, total organic carbon (TOC), combustion, heated persulfate or UV persulfate oxidation.

49. SM 5520 (B,F)-2011, oil and grease, hexane extractable material (HEM): n-hexane extraction and gravimetry, silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry.

50. SM 5530 (B,D)-2010, phenols, manual distillation, followed by colorimetric (4AAP) manual.

51. SM 5540 C-2011, surfactants, colorimetric (methylene blue).

The following changes would apply to Table IC at 40 CFR part 136:

1. SM 6200 (B,C)-2011, volatile organic compounds, purge and trap capillary-column gas chromatographic/mass spectrometric (GC/MS), purge and trap capillary-column gas chromatographic (GC).

2. SM 6440 B-2005, polynuclear aromatic hydrocarbons (PAHs), high performance liquid chromatography (HPLC).

The following changes would apply to Table ID at 40 CFR part 136:

1. SM 6630 (B, C)-2007, organochlorine pesticides, gas chromatography (GC).

2. SM 6640 B-2006, acidic herbicide compounds, gas chromatography (GC).

EPA also proposes revisions to certain Standard Methods approved in Part 136 for which Standard Methods adopted updates that contain substantive changes. The following summarizes these changes for each method, organized by the table at 40 CFR part 136 in which they appear.

The following changes would apply to Table IA and/or Table IH at 40 CFR part 136:

1. EPA proposes that the membrane filtration method SM 9222 B-1997 be replaced with SM 9222 B-2006. This method analyzes Coliform (total) in the presence of chlorine. The newer method includes a number of technology updates that do not significantly change the procedure. In addition, the method:

a. Modified the procedure to allow for the use of a humidified incubator if loose-lidded plates are used during incubation.

b. Added a note that five typical and five atypical colonies per membrane need to be identified during coliform verification.

c. Moved the definition of “Coliform” that was Section 4 of SM 9222, and renumbered the rest of the document, such that the “Procedure” is now Section 4, instead of Section 5. This is not a substantive change except that in Table IA, Parameter 4 “Coliform (total), in presence of chlorine, number per 100 mL” the citation for “MF with enrichment” would be changed from “9222 (B+B.5c)-1997” to “9222 (B+B.4c)-2006.”

2. EPA proposes that the membrane filtration method SM 9222 D-1997 be replaced with SM 9222 D-2006. This method analyzes Coliform (fecal) and Coliform (fecal) in the presence of chlorine. The new method allows use of a dry recirculating incubator as specified in the culture dishes section. In addition, EPA proposes to add the following footnote to Tables IA and IH regarding SM9222D-2006 for fecal coliform verification frequency: “The verification frequency is at least five typical and five atypical colonies per sampling site on the day of sample collection & analysis.” SM 9222 D-2006 specifies that the fecal coliform colonies should be verified “at a frequency established by the laboratory,” which can be as low as zero. Colonies need be verified to prevent misidentification of results as false positive or false negative.

3. EPA proposes that the membrane filtration method SM 9222 G-1997 be replaced with SM 9222 G-2006 in Table IH. These methods analyze for
E. coli
and Fecal Coliforms. The newer method includes a number of technology updates that do not significantly change the procedure. In addition, the method now has a modified composition of EC broth to include different quantities of KH
2
PO
4
and 4-methylumbelliferyl-β-D-glucuronide.

The following changes would apply to Table IB at 40 CFR part 136:

EPA proposes SM 2120 F-2011 be added to Table IB for Color. EPA previously approved it as SM 2120 E-1993. It is also similar to the currently approved National Council for Air and Stream Improvement, Inc. method that uses American Dye Manufacturers Institute weighted-ordinate spectrophotometric parameters.

1. EPA proposes that SM 3113 B-2004, a metals atomic absorption furnace method, be replaced with the revised version SM 3113 B-2010. The only substantive change would be a reduction in the required replicate analyses of each calibration standard from three to two. Similar EPA methods do not require replicates of each calibration standard.

Finally, Standard Methods requested that EPA propose SM 6810 for the analysis of pharmaceutical and personal care products in water. EPA does not propose to add this method because no supporting data were received by the deadline to demonstrate that the method had undergone full inter-laboratory validation.

D. Changes to 40 CFR 136.3 to Include New Versions of Approved ASTM Methods

EPA proposes to approve new versions of currently approved ASTM methods, for the same reasons outlined in the first paragraph of Section IV.B above. Many of the changes EPA proposes to ASTM Methods approved in 40 CFR part 136 do not contain any substantive changes. The following describes the proposed changes related to ASTM Methods in 40 CFR part 136. Each entry contains (in the following order): proposed ASTM method number and date, the parameter, a brief description of the analytical technique, and a brief description of any substantive changes in this revision from the last approved version of the method. The methods listed below are organized according to the table at 40 CFR part 136 in which they appear.

The following changes would apply to Table IB at 40 CFR part 136:

1. ASTM D 511-09 (A, B), calcium and magnesium, titrimetric (EDTA), AA direct aspiration; the modified method includes less specific calibration requirements for the part A titrimetric method than the previous version. However, the revised requirements are still more comprehensive than other approved methods. Therefore, EPA considers this revised method has adequate calibration criteria.

2. ASTM D 516-11, sulfate ion, turbidimetric, no substantive changes.

3. ASTM D 858-12 (A-C), manganese, atomic absorption (AA) direct aspiration, AA furnace; the modified method allows for pH adjustments in the laboratory, if the sample is returned within 14 days following sampling. The modified method also allows the use of block digestion systems for trace metal analysis, and quality control procedures now require the lab to analyze a continuing calibration blank and continuing calibration verification at a frequency of 10%.

4. ASTM D 859-10, silica, colorimetric, manual; the modified method allows the use of direct reading spectrophotometer or filter photometer, which is common for most approved colorimetric methods.

5. ASTM D 1067-11, acidity or alkalinity, electrometric endpoint or phenolphthalein endpoint; electrometric or colorimetric titration to pH 4.5, manual; no substantive changes

6. ASTM D 1068-10 (A-C), iron, AA direct aspiration; AA furnace; Colorimetric (Phenanthroline); EPA originally approved Parts A-D, but ASTM discontinued Part B. EPA proposes that Parts C and D in the existing 40 CFR part 136 Table 1B, be shifted to Parts B and C to account for the discontinued Part B. Additionally, ASTM increased the frequency of quality control parameters for Test Method A—Atomic Absorption. The method now includes a method blank, a matrix spike sample and a control sample with every ten samples.

7. ASTM D 1126-12, hardness, titrimetric (EDTA); no substantive changes.

8. ASTM D 1179-10, fluoride ion, electrode, manual; colorimetric, (SPADNS); The revision removed calculation, precision and bias, and quality control procedures (method blank, matrix spike, LCS) previously included for Test Method B-Ion Selective Electrode. The method replaces those requirements with a lab duplicate and a reference sample analysis. This is similar to EPA approved SM 4500-F
−
(C, D) currently in 40 CFR part 136. The revision also removed the silver sulfate reagent used to remove chloride from the sample, as it is no longer considered a major interference.

9. ASTM D 1246-10, bromide ion, electrode; no substantive changes.

10. ASTM D 1687-12 (A-C), chromium (total) and dissolved hexavalent chromium, colorimetric (diphenyl-carbazide); AA direct aspiration; AA furnace; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and now allows for pH adjustments in the laboratory if the sample is returned within 14 days following sampling.

11. ASTM D 1688-12 (A-C), copper, AA direct aspiration, AA furnace; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and now allows for pH adjustments in the laboratory if the sample is returned within 14 days following sampling. ASTM also requires analysis of a continuing calibration blank and continuing calibration verification at a 10% frequency.

12. ASTM D 1691-12 (A, B), zinc, AA direct aspiration; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and now allows for pH adjustments in the laboratory if the sample is returned within 14 days following sampling.

13. ASTM D 1976-12, dissolved, total-recoverable, or total elements, inductively coupled plasma/atomic emission spectroscopy (ICP/AES); ASTM modified the method to allow block digestion systems for trace metal analysis.

14. ASTM D 3223-12, total mercury, cold vapor, manual; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and requires analysis of a continuing calibration blank and continuing calibration verification at a 10% frequency.

15. ASTM D 3373-12, vanadium, AA furnace; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and requires analysis of a continuing calibration blank and continuing calibration verification at a 10% frequency. ASTM now allows for pH adjustments in the laboratory if the sample is returned within 14 days following sampling.

16. ASTM D 3557-12 (A-D), cadmium, AA direct aspiration, AA furnace, Voltammetry; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and requires analysis of a continuing calibration blank and continuing calibration verification at a 10% frequency. ASTM now allows for pH adjustments in the laboratory if the sample is returned within 14 days following sampling.

17. ASTM D 3590-11 (A, B), total Kjeldahl nitrogen, manual digestion and distillation or gas diffusion; semi-automated block digester colorimetric (distillation not required); ASTM revised the preservation method to allow storing samples at 2-6 °C, instead of the previous 4 °C. The method includes OI Analytical Flow Injection Analysis (FIA) performance data using an alternative copper sulfate catalyst in place of mercury (note: “OI Analytical” is a company name, not an acronym).

18. ASTM D 4382-12, barium, AA furnace; ASTM modified the method to allow the use of block digestion systems for trace metal analysis, and requires analysis of a continuing calibration blank and continuing calibration verification at a 10% frequency.

19. ASTM D 4658-09, sulfide ion, ion selective electrode; no substantive changes.

20. ASTM D 5257-11, dissolved hexavalent chromium, ion chromatography; ASTM recommends buffering samples containing very high levels of anionic species to a pH of 9-9.5, then filtering the sample and storing it at 11), followed by any of the following:

350.1, Rev. 2.0 (1993)

4500-NH
3
B-2011

973.49.
3

Nesslerization

D1426-08 (A)

973.49
3
, I-3520-85.
2

Titration

4500-NH
3
C-2011

Electrode

4500-NH
3
D-2011 or E-2011

D1426-08 (B)

Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods

4500-NH
3
F-2011

See footnote.
60

Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods

350.1
30
, Rev. 2.0 (1993)

4500-NH
3
G-2011

4500-NH
3
H-2011

I-4523-85.
2

Automated electrode

See footnote.
7

Ion Chromatography

D6919-09

Automated gas diffusion, followed by conductivity cell analysis

Timberline Ammonia-001
74

5. Antimony—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011

AA furnace

3113 B-2010

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

6. Arsenic-Total,
4
mg/L

Digestion
4
, followed by any of the following:

206.5 (Issued 1978)
1

AA gaseous hydride

3114 B-2011 or
3114 C-2011

D2972-08 (B)

I-3062-85.
2

AA furnace

3113 B-2010
D2972-08 (C)

I-4063-98.
49

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

Colorimetric (SDDC)

3500-As B-2011
D2972-08 (A)

I-3060-85.
2

7. Barium-Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 D-2011

I-3084-85.
2

AA furnace

3113 B-2010
D4382-12

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP
36

See footnote.
34

8. Beryllium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 D-2011 or 3111 E-2011
D3645-08 (A)

I-3095-85.
2

AA furnace

3113 B-2010
D3645-08 (B)

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP

D4190-08

See footnote.
34

Colorimetric (aluminon)

See footnote.
61

9. Biochemical oxygen demand (BOD5), mg/L
Dissolved Oxygen Depletion

5210 B-2011

973.44
3
, p. 17
9
, I-1578-78
8
, See footnote.
10, 63

10. Boron—Total,
37
mg/L

Colorimetric (curcumin)

4500-B B-2011

I-3112-85.
2

ICP/AES

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP

D4190-08

See footnote.
34

11. Bromide, mg/L
Electrode

D1246-10

I-1125-85.
2

Ion Chromatography
300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)
4110 B-2011, C-2011, D-2011
D4327-03

993.30.
3

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

12. Cadmium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011
or 3111 C-2011

D3557-12 (A or B)

974.27
3
, p. 37
9
, I-3135-85
2
or I-3136-85.
2

AA furnace

3113 B-2010
D3557-12 (D)

I-4138-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-1472-85
2
or I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP
36

D4190-08

See footnote.
34

Voltametry
11

D3557-12 (C)

Colorimetric (Dithizone)

3500-Cd-D-1990

13. Calcium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011
D511-09(B)

I-3152-85.
2

ICP/AES

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP

See footnote.
34

Titrimetric (EDTA)

3500-Ca B-2011
D511-09 (A)

Ion Chromatography

D6919-09

14. Carbonaceous biochemical oxygen demand (CBOD
5
), mg/L
12

Dissolved Oxygen Depletion with nitrification inhibitor

5210 B-2011

See footnote.
35, 63

15. Chemical oxygen demand (COD), mg/L
Titrimetric

410.3 (Rev. 1978)
1

5220 B-2011
or C-2011

D1252-06 (A)

973.46
3
, p. 17
9
, I-3560-85.
2

Spectrophotometric, manual or automatic
410.4, Rev. 2.0 (1993)
5220 D-2011
D1252-06 (B)

See footnotes.
13, 14
, I-3561-85.
2

16. Chloride, mg/L
Titrimetric: (silver nitrate)

4500-Cl
−
B-2011

D512-04 (B)

I-1183-85.
2

(Mercuric nitrate)

4500-Cl
−
C-2011

D512-04 (A)

973.51
3
, I-1184-85.
2

Colorimetric: manual

I-1187-85.
2

Automated (ferricyanide)

4500-Cl
−
E-2011

I-2187-85.
2

Potentiometric Titration

4500-Cl
−
D-2011

Ion Selective Electrode

D512-04 (C)

Ion Chromatography
300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)
4110 B-2011 or 4110 C-2011
D4327-03

993.30
3
, I-2057-90.
51

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

17. Chlorine—Total residual, mg/L
Amperometric direct

4500-Cl D-2011
D1253-08

Amperometric direct (low level)

4500-Cl E-2011

Iodometric direct

4500-Cl B-2011

Back titration ether end-point
15

4500-Cl C-2011

DPD-FAS

4500-Cl F-2011

Spectrophotometric, DPD

4500-Cl G-2011

Electrode

See footnote.
16

17A. Chlorine-Free Available, mg/L
Amperometric direct

4500-Cl D-2011
D1253-08

Amperometric direct (low level)

4500-Cl E-2011

DPD-FAS

4500-Cl F-2011

Spectrophotometric, DPD

4500-Cl G-2011

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

AA chelation-extraction

3111 C-2011

I-1232-85.
2

Ion Chromatography
218.6, Rev. 3.3 (1994)
3500-Cr C-2011
D5257-11
993.23.

Colorimetric (diphenyl-carbazide)

3500-Cr B-2011
D1687-12 (A)

I-1230-85.
2

19. Chromium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011
D1687-12 (B)

974.27
3
, I-3236-85.
2

AA chelation-extraction

3111 C-2011

AA furnace

3113 B-2010
D1687-12 (C)

I-3233-93.
46

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
, 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

DCP
36

D4190-08

See footnote.
34

Colorimetric (diphenyl-carbazide)

3500-Cr B-2011

20. Cobalt—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011 or 3111 C-2011
D3558-08 (A or B)

p. 37
9
, I-3239-85.
2

AA furnace

3113 B-2010
D3558-08 (C)

I-4243-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.7, Rev. 4.4 (1994)
3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

DCP

D4190-08

See footnote.
34

21. Color, platinum cobalt units or dominant wavelength, hue, luminance purity
Colorimetric (ADMI)

2120 F-2011

See footnote.
18

(Platinum cobalt) Spectrophotometric

2120 B-2011

I-1250-85.
2

22. Copper—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011 or
3111 C-2011

D1688-12 (A or B)

974.27
3
, p. 37
9
, I-3270-85
2
or I-3271-85.
2

AA furnace

3113 B-2010
D1688-12 (C)

I-4274-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

DCP
36

D4190-08

See footnote.
34

Colorimetric (Neocuproine)

3500-Cu B-2011

Colorimetric (Bathocuproine)

3500-Cu C-2011

See footnote.
19

23. Cyanide—Total, mg/L
Automated UV digestion/distillation and Colorimetry

Kelada-01.
55

Segmented Flow Injection, In-Line Ultraviolet Digestion, followed by gas diffusion amperometry

D7511-12

Manual distillation with MgCl
2
, followed by any of the following:

335.4, Rev. 1.0 (1993)
57

4500-CN
−
B-2011 and C-2011

D2036-09(A), D7284-13

10-204-00-1-X.
56

Flow Injection, gas diffusion amperometry

D2036-09(A) D7284-13

Titrimetric

4500-CN
−
D-2011

D2036-09(A)

p. 22.
9

Spectrophotometric, manual

4500-CN
−
E-2011

D2036-09(A)

I-3300-85.
2

Semi-Automated
20

335.4, Rev. 1.0 (1993)
57

10-204-00-1-X
56
, I-4302-85.
2

Ion Chromatography

D2036-09(A)

Ion Selective Electrode

4500-CN
−
F-2011

D2036-09(A)

24. Cyanide-Available, mg/L

Cyanide Amenable to Chlorination (CATC); Manual distillation with MgCl
2
, followed by Titrimetric or Spectrophotometric

4500-CN
−
G-2011

D2036-09(B)

Flow injection and ligand exchange, followed by gas diffusion amperometry
59

D6888-09

OIA-1677-09.
44

Automated Distillation and Colorimetry (no UV digestion)

Kelada-01.
55

24.A Cyanide-Free, mg/L
Flow Injection, followed by gas diffusion amperometry

D7237-10

OIA-1677-09.
44

Manual micro-diffusion and colorimetry

D4282-02

25. Fluoride—Total, mg/L

Manual distillation
6
, followed by any of the following:

4500-F
−
B-2011

Electrode, manual

4500-F
−
C-2011

D1179-10 (B)

Electrode, automated

I-4327-85.
2

Colorimetric, (SPADNS)

4500-F
−
D-2011

D1179-10 (A)

Automated complexone

4500-F
−
E-2011

Ion Chromatography
300.0, Rev 2.1 (1993) and 300.1-1, Rev 1.0 (1997)
4110 B-2011 or C-2011
D4327-03

993.30.
3

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

26. Gold—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

AA furnace

231.2 (Issued 1978)
1

3113 B-2010

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP

See footnote.
34

27. Hardness—Total, as CaCO
3
, mg/L

Automated colorimetric

130.1 (Issued 1971)
1

Titrimetric (EDTA)

2340 C-2011
D1126-12

973.52B
3
, I-1338-85.
2

Ca plus Mg as their carbonates, by any approved method for Ca and Mg (See Parameters 13 and 33), provided that the sum of the lowest point of quantitation for Ca and Mg is below the NPDES permit requirement for Hardness

2340 B-2011

28. Hydrogen ion (pH), pH units
Electrometric measurement

4500-H
+
B-2011

D1293-99 (A or B)

973.41
3
, I-1586-85.
2

Automated electrode

150.2 (Dec. 1982)
1

See footnote
21
, I-2587-85.
2

29. Iridium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

AA furnace

235.2 (Issued 1978)
1

ICP/MS

3125 B-2011

30. Iron—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011 or
3111 C-2011

D1068-10 (A)

974.27
3
, I-3381-85.
2

AA furnace

3113 B-2010
D1068-10 (B)

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP
36

D4190-08

See footnote.
34

Colorimetric (Phenanthroline)

3500-Fe-2011
D1068-10 (C)

See footnote.
22

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

Manual digestion
20
and distillation or gas diffusion, followed by any of the following:

4500-N
org
B-2011 or C-2011 and 4500-NH
3
B-2011

D3590-11 (A)

I-4515-91.
45

Titration

4500-NH
3
C-2011

973.48.
3

Nesslerization

D1426-08 (A)

Electrode

4500-NH
3
D-2011 or E-2011

D1426-08 (B)

Semi-automated phenate
350.1, Rev. 2.0 (1993)

4500-NH
3
G-2011

4500-NH
3
H-2011

Manual phenate, salicylate, or other substituted phenols in Berthelot reaction based methods

4500-NH
3
F-2011

See footnote.
60

Automated Methods for TKN that do not require manual distillation.

Automated phenate, salicylate, or other substituted phenols in Berthelot reaction based methods colorimetric (auto digestion and distillation)

351.1 (Rev. 1978)
1

I-4551-78.
8

Semi-automated block digestor colorimetric (distillation not required)
351.2, Rev. 2.0 (1993)

4500-N
org
D-2011

D3590-11 (B)

I-4515-91
45

Block digester, followed by Auto distillation and Titration

See footnote.
39

Block digester, followed by Auto distillation and Nesslerization

See footnote.
40

Block Digester, followed by Flow injection gas diffusion (distillation not required)

See footnote.
41

Digestion with peroxdisulfate, followed by Spectrophotometric (2,6-dimethyl phenol)

Hach 10242.
75

Digestion with persulfate, followed by Colorimetric

NCASI TNTP W10900.
77

32. Lead—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011 or 3111 C-2011.
D3559-08 (A or B)

974.27
3
, I-3399-85.
2

AA furnace

3113 B-2010
D3559-08 (D)

I-4403-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP
36

D4190-08

See footnote.
34

Voltametry
11

D3559-08 (C)

Colorimetric (Dithizone)

3500-Pb B-2011

33. Magnesium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011
D511-09 (B)

974.27
3
, I-3447-85.
2

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP

See footnote.
34

Ion Chromatography

D6919-09

34. Manganese—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011
D858-12 (A or B)

974.27
3
, I-3454-85.
2

AA furnace

3113 B-2010
D858-12 (C)

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP
36

D4190-08

See footnote.
34

Colorimetric (Persulfate)

3500-Mn B-2011

920.203.
3

Colorimetric (Periodate)

See footnote.
23

35. Mercury—Total,
4
mg/L

Cold vapor, Manual
245.1, Rev. 3.0 (1994)
3112 B-2011
D3223-12

977.22
3
, I-3462-85.
2

Cold vapor, Automated

245.2 (Issued 1974)
1

Cold vapor atomic fluorescence spectrometry (CVAFS)

245.7 Rev. 2.0 (2005)
17

I-4464-01.
71

Purge and Trap CVAFS

1631E
43

36. Molybdenum—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 D-2011

I-3490-85.
2

AA furnace

3113 B-2010

I-3492-96.
47

ICP/AES
36

200.7, Rev. 4.4 (1994)
3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP

See footnote.
34

37. Nickel—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011 or
3111 C-2011

D1886-08 (A or B)

I-3499-85.
2

AA furnace

3113 B-2010
D1886-08 (C)

I-4503-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

DCP
36

D4190-08

See footnote.
34

38. Nitrate (as N), mg/L
Ion Chromatography
300.0, Rev. 2.1 (1993) and 300.1-1, Rev. 1.0 (1997)
4110 B-2011 or C-2011
D4327-03

993.30.
3

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

Ion Selective Electrode

4500-NO
3

−
D-2011

Colorimetric (Brucine sulfate)

352.1 (Issued 1971)
1

973.50
3
, 419D
1,7
, p. 28.
9

Spectrophotometric (2,6-dimethylphenol)

Hach 10206.
75

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

See footnote.
62

Enzymatic reduction, followed by automated colorimetric determination

I-2547-11.
72

I-2548-11.
72

N07-0003.
73

39. Nitrate-nitrite (as N), mg/L
Cadmium reduction, Manual

4500-NO
3

−
E-2011

D3867-04 (B)

Cadmium reduction, Automated
353.2, Rev. 2.0 (1993)

4500-NO
3

−
F-2011

D3867-04 (A)

I-2545-90.
51

Automated hydrazine

4500-NO
3

−
H-2011

Reduction/Colorimetric

See footnote.
62

Ion Chromatography
300.0, Rev. 2.1 (1993) and 300.1-1, Rev. 1.0 (1997)
4110 B-2011 or C-2011
D4327-03

993.30.
3

CIE/UV

4140 B-2011
D6508-10

D6508, Rev. 2.
54

Enzymatic reduction, followed by automated colorimetric determination

I-2547-11.
72

I-2548-11.
72

N07-0003.
73

Spectrophotometric (2,6-dimethylphenol)

Hach 10206.
75

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

4500-NO
2

−
B-2011

See footnote.
25

Automated (Diazotization)

I-4540-85
2
, See footnote.
62

Automated (*bypass cadmium reduction)
353.2, Rev. 2.0 (1993)

4500-NO
3

−
F-2011

D3867-04 (A)

I-4545-85.
2

Manual (*bypass cadmium reduction)

4500-NO
3

−
E-2011

D3867-04 (B)

Ion Chromatography
300.0, Rev. 2.1 (1993) and 300.1-1, Rev. 1.0 (1997)
4110 B-2011 or C-2011
D4327-03

993.30.
3

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

Enzymatic reduction, followed by automated colorimetric determination

I-2547-11.
72

I-2548-11.
72

N07-0003.
73

41. Oil and grease—Total recoverable, mg/L
Hexane extractable material (HEM): n-Hexane extraction and gravimetry

1664 Rev. A; 1664 Rev. B
42

5520 B-2011
38

Silica gel treated HEM (SGT-HEM): Silica gel treatment and gravimetry

1664 Rev. A; 1664 Rev. B
42

5520 B-2011
38
and 5520 F-2011
38

42. Organic carbon—Total (TOC), mg/L
Combustion

5310 B-2011
D7573-09

973.47
3
, p. 14.
24

Heated persulfate or UV persulfate oxidation

5310 C-2011
5310 D-2011

D4839-03

973.47
3,
, p. 14.
24

43. Organic nitrogen (as N), mg/L
Total Kjeldahl N (Parameter 31) minus ammonia N (Parameter 4)

44. Ortho-phosphate (as P), mg/L
Ascorbic acid method:

Automated
365.1, Rev. 2.0 (1993)
4500-P F-2011 or G-2011

973.56
3
, I-4601-85.
2

Manual single reagent

4500-P E-2011
D515-88 (A)

973.55.
3

Manual two reagent

365.3 (Issued 1978)
1

Ion Chromatography
300.0, Rev. 2.1 (1993) and 300.1-1, Rev. 1.0 (1997)
4110 B-2011 or C-2000
D4327-03

993.30.
3

CIE/UV

4140 B-2011

D6508-10, D6508, Rev. 2
54

45. Osmium—Total
4
, mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 D-2011

AA furnace

252.2 (Issued 1978)
1

46. Oxygen, dissolved, mg/L
Winkler (Azide modification)

4500-O (B-F)-2011
D888-09 (A)

973.45B
3
, I-1575-78.
8

Electrode

4500-O G-2011
D888-09 (B)

I-1576-78.
8

Luminescence Based Sensor

D888-09 (C)

See footnote.
63

See footnote.
64

47. Palladium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

AA furnace

253.2 (Issued 1978)
1

ICP/MS

3125 B-2011

DCP

See footnote.
34

48. Phenols, mg/L

Manual distillation
26
, followed by any of the following:

420.1 (Rev. 1978)
1

5530 B-2010
D1783-01

Colorimetric (4AAP) manual

420.1 (Rev. 1978)
1

5530 D-2010
27

D1783-01 (A or B)

Automated colorimetric (4AAP)
420.4 Rev. 1.0 (1993)

49. Phosphorus (elemental), mg/L
Gas-liquid chromatography

See footnote.
28

50. Phosphorus—Total, mg/L

Digestion
20
, followed by any of the following:

4500-P B(5)-2011

973.55.
3

Manual

365.3 (Issued 1978)
1

4500-P E-2011
D515-88 (A)

Automated ascorbic acid reduction
365.1 Rev. 2.0 (1993)
4500-P (F-H)-2011

973.56
3
, I-4600-85.
2

ICP/AES
4, 36

200.7, Rev. 4.4 (1994)
3120 B-2011

I-4471-97.
50

Semi-automated block digestor (TKP digestion)

365.4 (Issued 1974)
1

D515-88 (B)

I-4610-91.
48

Digestion with persulfate, followed by Colorimetric

NCASI TNTP W10900.
77

51. Platinum—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

AA furnace

255.2 (Issued 1978)
1

ICP/MS

3125 B-2011

DCP

See footnote.
34

52. Potassium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

973.53
3
, I-3630-85.
2

ICP/AES
200.7, Rev. 4.4 (1994)
3120 B-2011

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

Flame photometric

3500-K B-2011

Electrode

3500-K C-2011

Ion Chromatography

D6919-09

53. Residue—Total, mg/L
Gravimetric, 103-105°

2540 B-2011

I-3750-85.
2

54. Residue—filterable, mg/L
Gravimetric, 180°

2540 C-2011
D5907-13

I-1750-85.
2

55. Residue—non-filterable (TSS), mg/L
Gravimetric, 103-105° post washing of residue

2540 D-2011
D5907-13

I-3765-85.
2

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

2540 F-2011

57. Residue—Volatile, mg/L
Gravimetric, 550°

160.4 (Issued 1971)
1

2540-E-2011

I-3753-85.
2

58. Rhodium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration, or

3111 B-2011

AA furnace

265.2 (Issued 1978)
1

ICP/MS

3125 B-2011

59. Ruthenium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration, or

3111 B-2011

AA furnace

267.2
1

ICP/MS

3125 B-2011

60. Selenium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA furnace

3113 B-2010
D3859-08 (B)

I-4668-98.
49

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
36

200.5, Rev 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

AA gaseous hydride

3114 B-2011, or 3114 C-2011
D3859-08 (A)

I-3667-85.
2

61. Silica—Dissolved,
37
mg/L

0.45-micron filtration followed by any of the following:

Colorimetric, Manual

4500-SiO
2
C-2011

D859-10

I-1700-85.
2

Automated (Molybdosilicate)

4500-SiO
2
E-2011 or F-2011

I-2700-85.
2

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

62. Silver—Total,
4

31
mg/L

Digestion
4, 29
, followed by any of the following:

AA direct aspiration

3111 B-2011 or
3111 C-2011

974.27
3
, p. 37
9
, I-3720-85.
2

AA furnace

3113 B-2010

I-4724-89.
51

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

DCP

See footnote.
34

63. Sodium—Total,
4
mg/L

Digestion
4,
, followed by any of the following:

AA direct aspiration

3111 B-2011

973.54
3
, I-3735-85.
2

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP

See footnote.
34

Flame photometric

3500-Na B-2011

Ion Chromatography

D6919-09

64. Specific conductance, micromhos/cm at 25 °C
Wheatstone bridge

120.1 (Rev. 1982)
1

2510 B-2011
D1125-95(99) (A)

973.40
3
, I-2781-85.
2

65. Sulfate (as SO
4
), mg/L

Automated colorimetric
375.2, Rev. 2.0 (1993)

4500-SO
4

2
−
F-2011 or G-2011

Gravimetric

4500-SO
4

2−
C-2011 or D-2011

925.54.
3

Turbidimetric

4500-SO
4

2−
E-2011

D516-11

Ion Chromatography
300.0, Rev. 2.1 (1993) and 300.1-1, Rev. 1.0 (1997)
4110 B-2011 or C-2011
D4327-03

993.30
3
, I-4020-05.
70

CIE/UV

4140 B-2011
D6508-1010

D6508, Rev. 2.
54

66. Sulfide (as S), mg/L
Sample Pretreatment

4500-S
2−>
B, C-2011

Titrimetric (iodine)

4500-S
2−
F-2011

I-3840-85.
2

Colorimetric (methylene blue)

4500-S
2−
D-2011

Ion Selective Electrode

4500-S
2−
G-2011

D4658-09

67. Sulfite (as SO
3
), mg/L

Titrimetric (iodine-iodate)

4500-SO
3

2−
B-2011

68. Surfactants, mg/L
Colorimetric (methylene blue)

5540 C-2011
D2330-02

69. Temperature, °C
Thermometric

2550 B-2010

See footnote.
32

70. Thallium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

AA furnace

279.2 (Issued 1978)
1

3113 B-2010

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES
200.7, Rev. 4.4 (1994)
3120 B-2011
D1976-12

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4471-97.
50

71. Tin—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 B-2011

I-3850-78.
8

AA furnace

3113 B-2010

STGFAA
200.9, Rev. 2.2 (1994)

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

72. Titanium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 D-2011

AA furnace

283.2 (Issued 1978)
1

ICP/AES
200.7, Rev. 4.4 (1994)

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14.
3

DCP

See footnote.
34

73. Turbidity, NTU
53

Nephelometric
180.1, Rev. 2.0 (1993)
2130 B-2011
D1889-00

I-3860-85.
2

See footnote.
65

See footnote.
66

See footnote.
67

74. Vanadium—Total,
4
mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration

3111 D-2011

AA furnace

3113 B-2010
D3373-12

ICP/AES

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05.
70

DCP

D4190-08

See footnote.
34

Colorimetric (Gallic Acid)

3500-V B-2011

75. Zinc—Total
4
, mg/L

Digestion
4
, followed by any of the following:

AA direct aspiration
36

3111 B-2011 or 3111 C-2011
D1691-12 (A or B)

974.27
3
, p. 37
9
, I-3900-85.
2

AA furnace

289.2 (Issued 1978)
1

ICP/AES
36

200.5, Rev. 4.2 (2003)
68
; 200.7, Rev. 4.4 (1994)

3120 B-2011
D1976-12

I-4471-97.
50

ICP/MS
200.8, Rev. 5.4 (1994)
3125 B-2011
D5673-10

993.14
3
, I-4020-05
70

DCP
36

D4190-08

See footnote.
34

Colorimetric (Zincon)

3500 Zn B-2011

See footnote.
33

76. Acid Mine Drainage

1627
69

Table IB Notes:

1
Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020. Revised March 1983 and 1979, where applicable. U.S. EPA.

2
Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resource Investigations of the U.S. Geological Survey, Book 5, Chapter A1., unless otherwise stated. 1989. USGS.

3
Official Methods of Analysis of the Association of Official Analytical Chemists, Methods Manual, Sixteenth Edition, 4th Revision, 1998. AOAC International.

4
For the determination of total metals (which are equivalent to total recoverable metals) the sample is not filtered before processing. A digestion procedure is required to solubilize analytes in suspended material and to break down organic-metal complexes (to convert the analyte to a detectable form for colorimetric analysis). For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid (as specified in Section 4.1.3 of Methods for the Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to gentle, acid refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids) digestion is preferred prior to analysis. The approved total recoverable digestion is described as Method 200.2 in Supplement I of “Methods for the Determination of Metals in Environmental Samples” EPA/600R-94/111, May, 1994, and is reproduced in EPA Methods 200.7, 200.8, and 200.9 from the same Supplement. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases the referenced method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct current plasma (DCP) technique or EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) use EPA Method 200.2 or an approved alternate procedure (
e.g.,
CEM microwave digestion, which may be used with certain analytes as indicated in Table IB); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods. Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as “total” metals.

5
Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.

6
Manual distillation is not required if comparability data on representative effluent samples are on file to show that this preliminary distillation step is not necessary: however, manual distillation will be required to resolve any controversies. In general, the analytical method should be consulted regarding the need for distillation. If the method is not clear, the laboratory may compare a minimum of 9 different sample matrices to evaluate the need for distillation. For each matrix, a matrix spike and matrix spike duplicate are analyzed both with and without the distillation step. (A total of 36 samples, assuming 9 matrices). If results are comparable, the laboratory may dispense with the distillation step for future analysis. Comparable is defined as 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 NH
4
OH. Add 1 mL of the cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.

32
”Water Temperature-Influential Factors, Field Measurement and Data Presentation,” Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1. 1975. USGS.

33
Method 8009, Zincon Method for Zinc, Hach Handbook of Water Analysis, 1979. Hach Company.

34
Method AES0029, Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes. 1986—Revised 1991. Thermo Jarrell Ash Corporation.

35
In-Situ Method 1004-8-2009, Carbonaceous Biochemical Oxygen Demand (CBOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.

36
Microwave-assisted digestion may be employed for this metal, when analyzed by this methodology. Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals. April 16, 1992. CEM Corporation

37
When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.

38
Only use n-hexane (n-Hexane—85% minimum purity, 99.0% min. saturated C6 isomers, residue less than 1 mg/L) extraction solvent when determining Oil and Grease parameters—Hexane Extractable Material (HEM), or Silica Gel Treated HEM (analogous to EPA Methods 1664 Rev. A and 1664 Rev. B). Use of other extraction solvents is prohibited.

39
Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical.

40
Method PAI-DK02, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Colorimetric Detection. Revised December 22, 1994. OI Analytical.

41
Method PAI-DK03, Nitrogen, Total Kjeldahl, Block Digestion, Automated FIA Gas Diffusion. Revised December 22, 1994. OI Analytical.

42
Method 1664 Rev. B is the revised version of EPA Method 1664 Rev. A. U.S. EPA. February 1999, Revision A. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-98-002. U.S. EPA. February 2010, Revision B. Method 1664, n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction and Gravimetry. EPA-821-R-10-001.

43
Method 1631, Revision E, Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-02-019. Revision E. August 2002, U.S. EPA. The application of clean techniques described in EPA's Method 1669:
Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels,
EPA-821-R-96-011, are recommended to preclude contamination at low-level, trace metal determinations.

44
Method OIA-1677-09, Available Cyanide by Ligand Exchange and Flow Injection Analysis (FIA). 2010. OI Analytical.

45
Open File Report 00-170, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion. 2000. USGS.

46
Open File Report 93-449, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry. 1993. USGS.

47
Open File Report 97-198, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum by Graphite Furnace Atomic Absorption Spectrophotometry. 1997. USGS.

48
Open File Report 92-146, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis. 1992. USGS.

49
Open File Report 98-639, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace-Atomic Absorption Spectrometry. 1999. USGS.

50
Open File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry. 1998. USGS.

51
Open File Report 93-125, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

52
Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1-1, are published in U.S. EPA. May 1994. Methods for the Determination of Metals in Environmental Samples, Supplement I, EPA/600/R-94/111; or U.S. EPA. August 1993. Methods for the Determination of Inorganic Substances in Environmental Samples, EPA/600/R-93/100. EPA Method 300.1 is US EPA. Revision 1.0, 1997, including errata cover sheet April 27, 1999. Determination of Inorganic Ions in Drinking Water by Ion Chromatography.

53
Styrene divinyl benzene beads (
e.g.,
AMCO-AEPA-1 or equivalent) and stabilized formazin (
e.g.,
Hach StablCal
TM
or equivalent) are acceptable substitutes for formazin.

54
Method D6508-10, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte. 2010. ASTM.

55
Kelada-01, Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, and Thiocyanate, EPA 821-B-01-009, Revision 1.2, August 2001. US EPA. Note: A 450-W UV lamp may be used in this method instead of the 550-W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met.

56
QuikChem Method 10-204-00-1-X, Digestion and Distillation of Total Cyanide in Drinking and Wastewaters using MICRO DIST and Determination of Cyanide by Flow Injection Analysis. Revision 2.2, March 2005. Lachat Instruments.

57
When using sulfide removal test procedures described in EPA Method 335.4-1, reconstitute particulate that is filtered with the sample prior to distillation.

58
Unless otherwise stated, if the language of this table specifies a sample digestion and/or distillation “followed by” analysis with a method, approved digestion and/or distillation are required prior to analysis.

59
Samples analyzed for available cyanide using OI Analytical method OIA-1677-09 or ASTM method D6888-09 that contain particulate matter may be filtered only after the ligand exchange reagents have been added to the samples, because the ligand exchange process converts complexes containing available cyanide to free cyanide, which is not removed by filtration. Analysts are further cautioned to limit the time between the addition of the ligand exchange reagents and sample filtration to no more than 30 minutes to preclude settling of materials in samples.

60
Analysts should be aware that pH optima and chromophore absorption maxima might differ when phenol is replaced by a substituted phenol as the color reagent in Berthelot Reaction (“phenol-hypochlorite reaction”) colorimetric ammonium determination methods. For example when phenol is used as the color reagent, pH optimum and wavelength of maximum absorbance are about 11.5 and 635 nm, respectively—see, Patton, C.J. and S.R. Crouch. March 1977. Anal. Chem. 49:464-469. These reaction parameters increase to pH > 12.6 and 665 nm when salicylate is used as the color reagent—see, Krom, M.D. April 1980. The Analyst 105:305-316.

61
If atomic absorption or ICP instrumentation is not available, the aluminon colorimetric method detailed in the 19th Edition of
Standard Methods
may be used. This method has poorer precision and bias than the methods of choice.

62
Easy (1-Reagent) Nitrate Method, Revision November 12, 2011. Craig Chinchilla.

63
Hach Method 10360, Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD
5
and cBOD
5.
Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB for measurement of biochemical oxygen demand (BOD) and carbonaceous biochemical oxygen demand (CBOD).

64
In-Situ Method 1002-8-2009, Dissolved Oxygen (DO) Measurement by Optical Probe. 2009. In-Situ Incorporated.

65
Mitchell Method M5331, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

66
Mitchell Method M5271, Determination of Turbidity by Nephelometry. Revision 1.0, July 31, 2008. Leck Mitchell.

67
Orion Method AQ4500, Determination of Turbidity by Nephelometry. Revision 5, March 12, 2009. Thermo Scientific.

68
EPA Method 200.5, Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry, EPA/600/R-06/115. Revision 4.2, October 2003. US EPA.

69
Method 1627, Kinetic Test Method for the Prediction of Mine Drainage Quality, EPA-821-R-09-002. December 2011. US EPA.

70
Techniques and Methods Book 5-B1, Determination of Elements in Natural-Water, Biota, Sediment and Soil Samples Using Collision/Reaction Cell Inductively Coupled Plasma-Mass Spectrometry, Chapter 1, Section B, Methods of the National Water Quality Laboratory, Book 5, Laboratory Analysis, 2006. USGS.

71
Water-Resources Investigations Report 01-4132, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Organic Plus Inorganic Mercury in Filtered and Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence Spectrometry, 2001. USGS.

72
USGS Techniques and Methods 5-B8, Chapter 8, Section B, Methods of the National Water Quality Laboratory Book 5, Laboratory Analysis, 2011 USGS.

73
NECi Method N07-0003, Revision 9.0, March 2014, Method for Nitrate Reductase Nitrate-Nitrogen Analysis, The Nitrate Elimination Co., Inc.

74
Timberline Instruments, LLC Method Ammonia-001, Timberline Instruments, LLC.

75
Hach Company Method 10206, Hach Company.

76
Hach Company Method 10242, Hach Company.

77
National Council for Air and Stream Improvement (NCASI) Method TNTP-W10900, Total (Kjeldahl) Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion. June 2011.

Table IC—List of Approved Test Procedures for Non-Pesticide Organic Compounds

Parameter
1

Method

EPA
2

7

Standard
methods

ASTM
Other

1. Acenaphthene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

2. Acenaphthylene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

3. Acrolein
GC
603

GC/MS

624.1
4
,1624B

4. Acrylonitrile
GC
603

GC/MS

624.1
4
,1624B

5. Anthracene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440B-2005
D4657-92 (98)

6. Benzene
GC
602
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

7. Benzidine
Spectro-photometric

See footnote
3
, p.1.

GC/MS

625.1
5
, 1625B

6410 B-2000

HPLC
605

8. Benzo(a)anthracene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

9. Benzo(a)pyrene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

10. Benzo(b)fluoranthene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

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

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

12. Benzo(k)fluoranthene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

13. Benzyl chloride
GC

See footnote
3
, p. 130.

GC/MS

See footnote
6
, p. S102.

14. Butyl benzyl phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

15. bis(2-Chloroethoxy) methane
GC
611

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

16. bis(2-Chloroethyl) ether
GC
611

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

17. bis(2-Ethylhexyl) phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

18. Bromodichloromethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

19. Bromoform
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

20. Bromomethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

21. 4-Bromophenyl phenyl ether
GC
611

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

22. Carbon tetrachloride
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

23. 4-Chloro-3-methyl phenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

24. Chlorobenzene
GC
601, 602
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

25. Chloroethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

26. 2-Chloroethylvinyl ether
GC
601

GC/MS
624.1, 1624B

27. Chloroform
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

28. Chloromethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

29. 2-Chloronaphthalene
GC
612

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

30. 2-Chlorophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

31. 4-Chlorophenyl phenyl ether
GC
611

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

32. Chrysene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

33. Dibenzo(a,h)anthracene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

34. Dibromochloromethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

35. 1,2-Dichlorobenzene
GC
601, 602
6200 C-2011

GC/MS
625.1, 1625B
6200 B-2011

See footnote
9
, p. 27.

36. 1,3-Dichlorobenzene
GC
601, 602
6200 C-2011

GC/MS
624.1, 1625B
6200 B-2011

See footnote
9
, p. 27.

37. 1,4-Dichlorobenzene
GC
601, 602
6200 C-2011

GC/MS
624.1, 1625B
6200 B-2011

See footnote
9
, p. 27.

38. 3,3′-Dichlorobenzidine
GC/MS
625.1, 1625B
6410 B-2000

HPLC
605

39. Dichlorodifluoromethane
GC
601

GC/MS

6200 C-2011

40. 1,1-Dichloroethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

41. 1,2-Dichloroethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

42. 1,1-Dichloroethene
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

43. trans-1,2-Dichloroethene
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

44. 2,4-Dichlorophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

45. 1,2-Dichloropropane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

46. cis-1,3-Dichloropropene
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

47. trans-1,3-Dichloropropene
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

48. Diethyl phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

49. 2,4-Dimethylphenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

50. Dimethyl phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

51. Di-n-butyl phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

52. Di-n-octyl phthalate
GC
606

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

53. 2, 4-Dinitrophenol
GC
604
6420 B-2000

See footnote
9
, p. 27.

GC/MS
625.1, 1625B
6410 B-2000

54. 2,4-Dinitrotoluene
GC
609

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

55. 2,6-Dinitrotoluene
GC
609

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

56. Epichlorohydrin
GC

See footnote
3
, p. 130.

GC/MS

See footnote
6
, p. S102.

57. Ethylbenzene
GC
602
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

58. Fluoranthene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

59. Fluorene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

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

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

62. 1,2,3,4,6,7,8- Heptachloro-dibenzo-
p
-dioxin

GC/MS
1613B

63. Hexachlorobenzene
GC
612

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

64. Hexachlorobutadiene
GC
612

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

65. Hexachlorocyclopentadiene
GC
612

GC/MS

625.1
5
, 1625B

6410 B-2000

See footnote
9
, p. 27.

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

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

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

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

70. 1,2,3,4,7,8-Hexachloro-dibenzo-
p
-dioxin

GC/MS
1613B

71. 1,2,3,6,7,8-Hexachloro-dibenzo-
p
-dioxin

GC/MS
1613B

72. 1,2,3,7,8,9-Hexachloro-dibenzo-
p
-dioxin

GC/MS
1613B

73. Hexachloroethane
GC
612

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

74. Indeno(1,2,3-c,d) pyrene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

75. Isophorone
GC
609

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

76. Methylene chloride
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

77. 2-Methyl-4,6-dinitrophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

78. Naphthalene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005

79. Nitrobenzene
GC
609

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC

D4657-92 (98)

80. 2-Nitrophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

81. 4-Nitrophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

82. N-Nitrosodimethylamine
GC
607

GC/MS

625.1
5
, 1625B

6410 B-2000

See footnote
9
, p. 27.

83. N-Nitrosodi-n-propylamine
GC
607

GC/MS

625.1
5
, 1625B

6410 B-2000

See footnote
9
, p. 27.

84. N-Nitrosodiphenylamine
GC
607

GC/MS

625.1
5
, 1625B

6410 B-2000

See footnote
9
, p. 27.

85. Octachlorodibenzofuran
GC/MS

1613B
10

86. Octachlorodibenzo-
p
-dioxin

GC/MS

1613B
10

87. 2,2′-oxybis(1-chloropropane)
12
[also known as bis(2-Chloro-1-methylethyl) ether]

GC
611

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

88. PCB-1016
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

89. PCB-1221
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

90. PCB-1232
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

91. PCB-1242
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

92. PCB-1248
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

93. PCB-1254
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

94. PCB-1260
GC
608.3

See footnote
3
, p. 43; See footnote.
8

GC/MS
625.1
6410 B-2000

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

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

97. 1,2,3,7,8,-Pentachloro-dibenzo-
p
-dioxin

GC/MS
1613B

98. Pentachlorophenol
GC
604
6420 B-2000

See footnote
3
, p. 140.

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

99. Phenanthrene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98)

100. Phenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

101. Pyrene
GC
610

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

HPLC
610
6440 B-2005
D4657-92 (98).

102. 2,3,7,8-Tetrachloro-dibenzofuran
GC/MS

1613B
10

103. 2,3,7,8-Tetrachloro-dibenzo-
p
-dioxin

GC/MS

613, 625.1
5a
, 1613B

104. 1,1,2,2-Tetrachloroethane
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

105. Tetrachloroethene
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

106. Toluene
GC
602
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

107. 1,2,4-Trichlorobenzene
GC
612

See footnote
3
, p. 130.

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

108. 1,1,1-Trichloroethane
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

109. 1,1,2-Trichloroethane
GC
601
6200 C-2011

See footnote
3
, p. 130.

GC/MS
624.1, 1624B
6200 B-2011

110. Trichloroethene
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

111. Trichlorofluoromethane
GC
601
6200 C-2011

GC/MS
624.1
6200 B-2011

112. 2,4,6-Trichlorophenol
GC
604
6420 B-2000

GC/MS
625.1, 1625B
6410 B-2000

See footnote
9
, p. 27.

113. Vinyl chloride
GC
601
6200 C-2011

GC/MS
624.1, 1624B
6200 B-2011

114. Nonylphenol
GC/MS

D7065-11

115. Bisphenol A (BPA)
GC/MS

D7065-11

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

D7065-11

117. Nonylphenol Monoethoxylate (NP1EO)
GC/MS

D7065-11

118. Nonylphenol Diethoxylate (NP2EO)
GC/MS

D7065-11

119. Adsorbable Organic Halides (AOX)
Adsorption and Coulometric Titration

1650
11

120. Chlorinated Phenolics
In Situ Acetylation and GC/MS

1653
11

Table IC notes:

1
All 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).

2
The full text of Methods 601-613, 1613B, 1624B, and 1625B are provided at Appendix A, Test Procedures for Analysis of Organic Pollutants, of this Part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, Definition and Procedure for the Determination of the Method Detection Limit, of this Part 136. Methods 608.3, 624.1, and 625.1 are available at:
water.epa.gov/scitech/methods/cwa/methods_index.cfm.

3
Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA.

4
Method 624.1 may be used for quantitative determination of acrolein and acrylonitrile, provided that the laboratory has documentation to substantiate the ability to detect and quantify these analytes at levels necessary to comply with any associated regulations. In addition, the use of sample introduction techniques other than simple purge-and-trap may be required. QC acceptance criteria from Method 603 should be used when analyzing samples for acrolein and acrylonitrile in the absence of such criteria in Method 624.1.

5
Method 625.1 may be extended to include benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, N-nitrosodi-n-propylamine, and N-nitrosodiphenylamine. However, when they are known to be present, Methods 605, 607, and 612, or Method 1625B, are preferred methods for these compounds.

5a
Method 625.1 screening only.

6
Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of
Standard Methods for the Examination of Water and Wastewater
1981. American Public Health Association (APHA).

7
Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 1624B, and 1625B in accordance with procedures each in Section 8.2 of each of these Methods. Additionally, each laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624.1 and 625.1 and 100% for methods 1624B and 1625B) of all samples to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

8
Organochlorine Pesticides and PCBs in Wastewater Using Empore
TM
Disk. Revised October 28, 1994. 3M Corporation.

9
Method O-3116-87 is in Open File Report 93-125, Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments. 1993. USGS.

10
Analysts may use Fluid Management Systems, Inc. Power-Prep system in place of manual cleanup provided the analyst meets the requirements of Method 1613B (as specified in Section 9 of the method) and permitting authorities. Method 1613, Revision B, Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS. Revision B, 1994. U.S. EPA. The full text of this method is provided in Appendix A to 40 CFR part 136 and at
http://water.epa.gov/scitech/methods/cwa/index.cfm.

11
Method 1650, Adsorbable Organic Halides by Adsorption and Coulometric Titration. Revision C, 1997 U.S. EPA. Method 1653, Chlorinated Phenolics in Wastewater by In Situ Acetylation and GCMS. Revision A, 1997 U.S. EPA. The full text for both of these methods is provided at Appendix A in part 430, The Pulp, Paper, and Paperboard Point Source Category.

12
The compound was formerly inaccurately labeled as 2,2′-oxybis(2-chloropropane) and bis(2-chloroisopropyl) ether. Some versions of Methods 611, and 1625 inaccurately list the analyte as “bis(2-chloroisopropyl)ether,” but use the correct CAS number of 108-60-1.

Table ID—List of Approved Test Procedures for Pesticides
1

Parameter
Method

EPA
2 7 10

Standard
methods

ASTM
Other

1. Aldrin
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96 (02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

2. Ametryn
GC
507, 619

See footnote,
3
p. 83; See footnote,
9
O-3106-93; See footnote,
6
p. S68.

GC/MS
525.2, 625.1

See footnote,
14
O-1121-91.

3. Aminocarb
TLC

See footnote,
3
p. 94; See footnote,
6
p. S60.

HPLC
632

4. Atraton
GC
619

See footnote,
3
p. 83; See footnote,
6
p. S68.

GC/MS
625.1

5. Atrazine
GC
507, 619, 608.3

See footnote,
3
p. 83; See footnote,
6
p. S68; See footnote,
9
O-3106-93.

HPLC/MS

See footnote,
12
O-2060-01.

GC/MS
525.1, 525.2, 625.1

See footnote,
11
O-1126-95.

6. Azinphos methyl
GC
614, 622, 1657

See footnote,
3
p. 25; See footnote,
6
p. S51.

GC-MS
625.1

See footnote,
11
O-1126-95.

7. Barban
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

GC/MS
625.1

8. α-BHC
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
8
3M0222.

GC/MS

625.1
5

6410 B-2000

See footnote,
11
O-1126-95.

9. β-BHC
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

10. δ-BHC
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

11. γ-BHC (Lindane)
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS

625.1
5

6410 B-2000

See footnote,
11
O-1126-95.

12. Captan
GC
617, 608.3
6630 B-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7.

13. Carbaryl
TLC

See footnote,
3
p. 94, See footnote,
6
p. S60.

HPLC
531.1, 632

HPLC/MS
553

See footnote,
12
O-2060-01.

GC/MS
625.1

See footnote,
11
O-1126-95.

14. Carbophenothion
GC
617, 608.3
6630 B-2007

See footnote,
4
page 27; See footnote,
6
p. S73.

GC/MS
625.1

15. Chlordane
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

16. Chloropropham
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

GC/MS
625.1

17. 2,4-D
GC
615
6640 B-2006

See footnote,
3
p. 115; See footnote,
4
O-3105-83.

HPLC/MS

See footnote,
12
O-2060-01.

18. 4,4′-DDD
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3105-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

19. 4,4′-DDE
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

See footnote,
11
O-1126-95.

20. 4,4′-DDT
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

21. Demeton-O
GC
614, 622

See footnote,
3
p. 25; See footnote,
6
p. S51.

GC/MS
625.1

22. Demeton-S
GC
614, 622

See footnote,
3
p. 25; See footnote,
6
p. S51.

GC/MS
625.1

23. Diazinon
GC
507, 614, 622, 1657

See footnote,
3
p. 25; See footnote,
4
O-3104-83; See footnote,
6
p. S51.

GC/MS
525.2, 625.1

See footnote,
11
O-1126-95.

24. Dicamba
GC
615

See footnote,
3
p. 115.

HPLC/MS

See footnote,
12
O-2060-01.

25. Dichlofenthion
GC
622.1

See footnote,
4
page 27; See footnote,
6
p. S73.

26. Dichloran
GC
608.2, 617, 608.3
6630 B-2007

See footnote,
3
p. 7;

27. Dicofol
GC
617, 608.3

See footnote,
4
O-3104-83.

28. Dieldrin
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

See footnote,
11
O-1126-95.

29. Dioxathion
GC
614.1, 1657

See footnote,
4
page 27; See footnote,
6
p. S73.

30. Disulfoton
GC
507, 614, 622, 1657

See footnote,
3
p. 25; See footnote,
6
p. S51.

GC/MS
525.2, 625.1

See footnote,
11
O-1126-95.

31. Diuron
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS
553

See footnote,
12
O-2060-01.

32. Endosulfan I
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS

625.1
5

6410 B-2000

See footnote,
13
O-2002-01.

33. Endosulfan II
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
8
3M0222.

GC/MS

625.1
5

6410 B-2000

See footnote,
13
O-2002-01.

34. Endosulfan Sulfate
GC
617, 608.3
6630 C-2007

See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

35. Endrin
GC
505, 508, 617, 1656, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS

525.1, 525.2, 625.1
5

6410 B-2000

36. Endrin aldehyde
GC
617, 608.3
6630 C-2007

See footnote,
8
3M0222.

GC/MS
625.1

37. Ethion
GC
614, 614.1,1657

See footnote,
4
page 27; See footnote,
6
p. S73.

GC/MS
625.1

See footnote,
13
O-2002-01.

38. Fenuron
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS

See footnote,
12
O-2060-01.

39. Fenuron-TCA
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

40. Heptachlor
GC
505, 508, 617, 1656, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
525.1, 525.2, 625.1
6410 B-2000

41. Heptachlor epoxide
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
6
p. S73; See footnote,
8
3M0222.

GC/MS
625.1
6410 B-2000

42. Isodrin
GC
617, 608.3
6630 B-2007 & C-2007

See footnote,
4
O-3104-83; See footnote,
6
p. S73.

GC/MS
625.1

43. Linuron
GC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS
553

See footnote,
12
O-2060-01.

GC/MS

Seeootnote,
11
O-1126-95.

44. Malathion
GC
614, 1657
6630 B-2007

See footnote,
3
p. 25; See footnote,
6
p. S51.

GC/MS
625.1

See footnote,
11
O-1126-95.

45. Methiocarb
TLC

See footnote,
3
p. 94; See footnote,
6
p. S60.

HPLC
632

HPLC/MS

See footnote,
12
O-2060-01.

46. Methoxychlor
GC
505, 508, 608.2, 617, 1656, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83; See footnote,
8
3M0222.

GC/MS
525.1, 525.2, 625.1

See footnote,
11
O-1126-95.

47. Mexacarbate
TLC

See footnote,
3
p. 94; See footnote,
6
p. S60.

HPLC
632

GC/MS
625.1

48. Mirex
GC
617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
4
O-3104-83.

GC/MS
625.1

49. Monuron
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

50. Monuron-TCA
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

51. Neburon
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS

See footnote,
12
O-2060-01.

52. Parathion methyl
GC
614, 622, 1657
6630 B-2007

See footnote,
4
page 27; See footnote,
3
p. 25.

GC/MS
625.1

See footnote,
11
O-1126-95.

53. Parathion ethyl
GC
614
6630 B-2007

See footnote,
4
page 27; See footnote,
3
p. 25.

GC/MS

See footnote,
11
O-1126-95.

54. PCNB
GC
608.1, 617, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7.

55. Perthane
GC
617, 608.3

D3086-90, D5812-96(02)

See footnote,
4
O-3104-83.

56. Prometon
GC
507, 619

See footnote,
3
p. 83; See footnote,
6
p. S68; See footnote,
9
O-3106-93.

GC/MS
525.2, 625.1

See footnote,
11
O-1126-95.

57. Prometryn
GC
507, 619

See footnote,
3
p. 83; See footnote,
6
p. S68; See footnote,
9
O-3106-93.

GC/MS
525.1, 525.2, 625.1

See footnote,
13
O-2002-01.

58. Propazine
GC
507, 619, 1656, 608.3

See footnote,
3
p. 83; See footnote,
6
p. S68; See footnote,
9
O-3106-93.

GC/MS
525.1, 525.2, 625.1

59. Propham
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS

See footnote,
12
O-2060-01.

60. Propoxur
TLC

See footnote,
3
p. 94; See footnote,
6
p. S60.

HPLC
632

61. Secbumeton
TLC

See footnote,
3
p. 83; See footnote,
6
p. S68.

GC
619

62. Siduron
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

HPLC/MS

See footnote,
12
O-2060-01.

63. Simazine
GC
505, 507, 619, 1656, 608.3

See footnote,
3
p. 83; See footnote,
6
p. S68; See footnote,
9
O-3106-93.

GC/MS
525.1, 525.2, 625.1

See footnote,
11
O-1126-95.

64. Strobane
GC
617, 608.3
6630 B-2007 & C-2007

See footnote,
3
p. 7.

65. Swep
TLC

See footnote,
3
p. 104; See footnote,
6
p. S64.

HPLC
632

66. 2,4,5-T
GC
615
6640 B-2006

See footnote,
3
p. 115; See footnote,
4
O-3105-83.

67. 2,4,5-TP (Silvex)
GC
615
6640 B-2006

See footnote,
3
p. 115; See footnote,
4
O-3105-83.

68. Terbuthylazine
GC
619, 1656, 608.3

See footnote,
3
p. 83; See footnote,
6
p. S68.

GC/MS

See footnote,
13
O-2002-01.

69. Toxaphene
GC
505, 508, 617, 1656, 608.3
6630 B-2007 & C-2007
D3086-90, D5812-96(02)

See footnote,
3
p. 7; See footnote,
8
; See footnote,
4
O-3105-83.

GC/MS
525.1, 525.2, 625.1
6410 B-2000

70. Trifluralin
GC
508, 617, 627, 1656, 608.3
6630 B-2007

See footnote,
3
p. 7; See footnote,
9
O-3106-93.

GC/MS
525.2, 625.1

See footnote,
11
O-1126-95.

Table ID notes:

1
Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC, where entries are listed by chemical name.

2
The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, Definition and Procedure for the Determination of the Method Detection Limit, of this Part 136.

3
Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA publication includes thin-layer chromatography (TLC) methods.

4
Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3. 1987. USGS.

5
The method may be extended to include α-BHC, γ-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist, Method 608.3 is the preferred method.

6
Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of
Standard Methods for the Examination of Water and Wastewater.
1981. American Public Health Association (APHA).

7
Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608.3 and 625.1 in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and analyze 5% of all samples analyzed with Method 608.3 or 5% of all samples analyzed with Method 625.1 to monitor and evaluate laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.

8
Organochlorine Pesticides and PCBs in Wastewater Using Empore
TM
Disk. Revised October 28, 1994. 3M Corporation.

9
Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography With Nitrogen Phosphorus Detectors. 1994. USGS.

10
EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA Method 525.2 is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass Spectrometry, Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA. Methods 608.3 and 625.1 are available at:
http://water.epa.gov/scitech/methods/cwa/methods_index.cfm
(this is a placeholder for now).

11
Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995. USGS.

12
Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry. 2001. USGS.

13
Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry. 2001. USGS.

14
Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1992. USGS.

Table 1F—List of Approved Methods for Pharmaceutical Pollutants

Pharmaceuticals pollutants
CAS Registry No.
Analytical method number

Acetonitrile
75-05-8
1666/1671/D3371/D3695/624.1.

n-Amyl acetate
628-63-7
1666/D3695.

n-Amyl alcohol
71-41-0
1666/D3695.

Benzene
71-43-2
D4763/D3695/502.2/524.2/624.1.

n-Butyl-acetate
123-86-4
1666/D3695.

tert
-Butyl alcohol

75-65-0
1666/624.1.

Chlorobenzene
108-90-7
502.2/524.2/624.1.

Chloroform
67-66-3
502.2/524.2/551/624.1.

o
-Dichlorobenzene

95-50-1
1625C/502.2/524.2/624.1.

1,2-Dichloroethane
107-06-2
D3695/502.2/524.2/624.1.

Diethylamine
109-89-7
1666/1671.

Dimethyl sulfoxide
67-68-5
1666/1671.

Ethanol
64-17-5
1666/1671/D3695/624.1.

Ethyl acetate
141-78-6
1666/D3695/624.1.

n-Heptane
142-82-5
1666/D3695.

n-Hexane
110-54-3
1666/D3695.

Isobutyraldehyde
78-84-2
1666/1667.

Isopropanol
67-63-0
1666/D3695.

Isopropyl acetate
108-21-4
1666/D3695.

Isopropyl ether
108-20-3
1666/D3695.

Methanol
67-56-1
1666/1671/D3695/624.1.

Methyl Cellosolve ® (2-Methoxy ethanol)
109-86-4
1666/1671.

Methylene chloride
75-09-2
502.2/524.2/624.1.

Methyl formate
107-31-3
1666.

4-Methyl-2-pentanone (MIBK)
108-10-1
1624C/1666/D3695/D4763/524.2/624.1.

Phenol
108-95-2
D4763.

n-Propanol
71-23-8
1666/1671/D3695/624.1.

2-Propanone (Acetone)
67-64-1
D3695/D4763/524.2/624.1.

Tetrahydrofuran
109-99-9
1666/524.2/624.1.

Toluene
108-88-3
D3695/D4763/502.2/524.2/624.1.

Triethlyamine
121-44-8
1666/1671.

Xylenes
(Note 1)
1624C/1666/624.1.

Table 1F note:

1
1624C:
m
-xylene 108-38-3,
o,p
-xylene, E-14095 (Not a CAS number; this is the number provided in the Environmental Monitoring Methods Index [EMMI] database.); 1666: m,p-xylene 136777-61-2,
o
-xylene 95-47-6.

Table 1G—Test Methods for Pesticide Active Ingredients (40 CFR part 455)

EPA survey code
Pesticide name
CAS No.

EPA analytical method No.(s)
3

8
Triadimefon
43121-43-3
507/633/525.1/525.2/1656/625.1.

12
Dichlorvos
62-73-7
1657/507/622/525.1/525.2/625.1.

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
1657/507/622/525.1/525.2/625.1.

25
Cyanazine
21725-46-2
629/507/608.3/625.1.

26
Propachlor
1918-16-7
1656/508/608.1/525.1/525.2/608.3/625.1.

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
525.1/525.2/507/633.1/625.1.

41
Propanil
709-98-8
632.1/1656/608.3.

45
Metribuzin
21087-64-9
507/633/525.1/525.2/1656/608.3/ 625.1.

52
Acephate
30560-19-1
1656/1657/608.3.

53
Acifluorfen
50594-66-6
515.1/515.2/555.

54
Alachlor
15972-60-8
505/507/645/525.1/525.2/1656/608.3/625.1.

55
Aldicarb
116-06-3
531.1.

58
Ametryn
834-12-8
507/619/525.2/625.1.

60
Atrazine
1912-24-9
505/507/619/525.1/525.2/1656/ 608.3/625.1.

62
Benomyl
17804-35-2
631.

68
Bromacil; Bromacil Salts and Esters
314-40-9
507/633/525.1/525.2/1656/608.3/ 625.1.

69
Bromoxynil
1689-84-5
1625/1661/625.1.

69
Bromoxynil octanoate
1689-99-2
1656/608.3.

70
Butachlor
23184-66-9
507/645/525.1/525.2/1656/608.3/625.1.

73
Captafol
2425-06-1
1656/608.3/625.1.

75
Carbaryl [Sevin]
63-25-2
531.1/632/553/625.1.

76
Carbofuran
1563-66-2
531.1/632/625.1.

80
Chloroneb
2675-77-6
1656/508/608.1/525.1/525.2/608.3/625.1.

82
Chlorothalonil
1897-45-6
508/608.2/525.1/525.2/1656/608.3/625.1.

84
Stirofos
961-11-5
1657/507/622/525.1/525.2/625.1.

86
Chlorpyrifos
2921-88-2
1657/508/622/625.1.

90
Fenvalerate
51630-58-1
1660.

103
Diazinon
333-41-5
1657/507/614/622/525.2/625.1.

107
Parathion methyl
298-00-0
1657/614/622/625.1.

110
DCPA [Dimethyl 2,3,5,6-tetrachloro-terephthalate]
1861-32-1

508/608.2/525.1/525.2/515.1
2
/515.2
2
/1656/608.3/625.1.

112
Dinoseb
88-85-7
1658/515.1/615/515.2/555/625.1.

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
1656/505/508/617/525.1/525.2/608.3/625.1.

125
Ethalfluralin
55283-68-6
1656/627/608.3 See footnote 1.

126
Ethion
563-12-2
1657/614/614.1/625.1.

127
Ethoprop
13194-48-4
1657/507/622/525.1/525.2/625.1.

132
Fenarimol
60168-88-9
507/633.1/525.1/525.2/1656/608.3/625.1.

133
Fenthion
55-38-9
1657/622/625.1.

138
Glyphosate [N-(Phosphonomethyl) glycine]
1071-83-6
547.

140
Heptachlor
76-44-8
1656/505/508/617/525.1/525.2/608.3/625.1.

144
Isopropalin
33820-53-0
1656/627/608.3.

148
Linuron
330-55-2
553/632.

150
Malathion
121-75-5
1657/614/625.1.

154
Methamidophos
10265-92-6
1657.

156
Methomyl
16752-77-5
531.1/632.

158
Methoxychlor
72-43-5
1656/505/508/608.2/617/525.1/525.2/608.3/625.1.

172
Nabam
142-59-6
630/630.1.

173
Naled
300-76-5
1657/622/625.1.

175
Norflurazon
27314-13-2
507/645/525.1/525.2/1656/608.3/625.1.

178
Benfluralin
1861-40-1
1656/627/608.3 See footnote 1.

182
Fensulfothion
115-90-2
1657/622/625.1.

183
Disulfoton
298-04-4
1657/507/614/622/525.2/625.1.

185
Phosmet
732-11-6
1657/622.1/625.1.

186
Azinphos Methyl
86-50-0
1657/614/622/625.1.

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
1657/614/625.1.

204
Pendimethalin
40487-42-1
1656.

205
Pentachloronitrobenzene
82-68-8
1656/608.1/617/608.3/625.1.

206
Pentachlorophenol
87-86-5
1625/515.2/555/515.1/525.1/525.2/625.1.

208
Permethrin
52645-53-1

608.2/508/525.1/525.2/1656/1660/608.3
4
/625.1
4
.

212
Phorate
298-02-2
1657/622/625.1.

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
507/619/525.2/625.1.

224
Prometryn
7287-19-6
507/619/525.1/525.2/625.1.

226
Propazine
139-40-2
507/619/525.1/525.2/1656/608.3/625.1.

230
Pyrethrin I
121-21-1
1660.

232
Pyrethrin II
121-29-9
1660.

236
DEF [S,S,S-Tributyl phosphorotrithioate]
78-48-8
1657.

239
Simazine
122-34-9
505/507/619/525.1/525.2/1656/608.3/625.1.

241
Carbam-S [Sodium dimethyldithio-carbamate]
128-04-1
630/630.1.

243
Vapam [Sodium methyldithiocarbamate]
137-42-8
630/630.1.

252
Tebuthiuron
34014-18-1
507/525.1/525.2/625.1.

254
Terbacil
5902-51-2
507/633/525.1/525.2/1656/608.3/625.1.

255
Terbufos
13071-79-9
1657/507/614.1/525.1/525.2/625.1.

256
Terbuthylazine
5915-41-3
619/1656/608.3.

257
Terbutryn
886-50-0
507/619/525.1/525.2/625.1.

259
Dazomet
533-74-4
630/630.1/1659.

262
Toxaphene
8001-35-2
1656/505/508/617/525.1/525.2/608.3/625.1.

263
Merphos [Tributyl phosphorotrithioate]
150-50-5
1657/507/525.1/525.2/622/625.1.

264

Trifluralin
1

1582-09-8
1656/508/617/627/525.2/608.3/625.1.

268
Ziram [Zinc dimethyldithiocarbamate]
137-30-4
630/630.1.

Table 1G notes:

1
Monitor and report as total Trifluralin.

2
Applicable to the analysis of DCPA degradates.

3
EPA Methods 608.1 through 645, 1645 through 1661, and Ind-01 are available in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume I, EPA 821-R-93-010A, Revision I, August 1993, U.S. EPA. EPA Methods 200.9 and 505 through 555 are available in Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, August 1993, U.S. EPA. The full text of Methods 608.3, 625.1, and 1625 are provided at Appendix A of this part 136. The full text of Method 200.7 is provided at Appendix C of this part 136. Methods 608.3 and 625.1 are available at:
http://water.epa.gov/scitech/methods/cwa/methods_index.cfm
(this is a placeholder for now).

4
Permethrin is not listed within methods 608.3 and 625.1; however, cis-permethrin and trans-permethrin are listed. Permethrin can be calculated by adding the results of cis and trans-permethrin.

Table 1H—List of Approved Microbiological Methods for Ambient Water

Parameter and units

Method
1

EPA
Standard methods
AOAC, ASTM, USGS
Other

Bacteria:

1. Coliform (fecal), number per 100 mL or number per gram dry weight
Most Probable Number (MPN), 5 tube, 3 dilution, or

p. 132
3

9221 C E-2006

Membrane filter (MF),
2
single step

p. 124
3

9222 D-2006
27

B-0050-85
4

2. Coliform (fecal) in presence of chlorine, number per 100 mL
MPN, 5 tube, 3 dilution, or

p. 132
3

9221 C E-2006

MF
2
, single step
5

p. 124
3

9222 D-2006
27

3. Coliform (total), number per 100 mL
MPN, 5 tube, 3 dilution, or

p. 114
3

9221 B-2006

MF
2
, single step or two step

p. 108
3

9222 B-2006

B-0025-85
4

4. Coliform (total), in presence of chlorine, number per 100 mL
MPN, 5 tube, 3 dilution, or

p. 114
3

9221 B-2006

MF
2
with enrichment

p. 111
3

9222 B-2006

5.
E. coli,
number per 100 mL

MPN,
6 8 14
multiple tube, or

9221 B.2-2006/9221 F-2006
11 13

Multiple tube/multiple well, or

9223 B-2004
12

991.15
10

Colilert®
12 16
, Colilert-®
12 15 16

MF
2 5 6 7 8
, two step, or

1103.1
19

9222 B-2006/9222 G-2006,
18
9213 D-2007

D5392-93
9

Single step

1603
20
, 1604
21

mColiBlue-24®
17

6. Fecal streptococci, number per 100 mL
MPN, 5 tube, 3 dilution, or

p. 139
3

9230 B-2007

MF
2
, or

p. 136
3

9230 C-2007

B-0055-85
4

Plate count

p. 143
3

7. Enterococci, number per 100 mL

MPN,
6 8
multiple tube/multiple well, or

9230 D-2007

D6503-99
9

Ente- rolert®
12 22

MF
2 5 6 7 8
two step, or

1106.1
23

9230 C-2007

D5259-92
9

Single step, or

1600
24

9230 C-2007

Plate count

p. 143
3

Protozoa:

8.
Cryptosporidium

Filtration/IMS/FA

1622
25
, 1623
26

9.
Giardia

Filtration/IMS/FA

1623
26

Table 1H notes:

1
The method must be specified when results are reported.

2
A 0.45-µm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of extractables which could interfere with their growth.

3
Microbiological Methods for Monitoring the Environment, Water, and Wastes. EPA/600/8-78/017. 1978. US EPA.

4
U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS.

5
Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.

6
Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.

7
When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.

8
To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.

9
Annual Book of ASTM Standards—Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.

10
Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.

11
The multiple-tube fermentation test is used in 9221B.2-2006. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.

12
These tests are collectively known as defined enzyme substrate tests, where, for exam

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Source: Frix Law Library, https://www.frixlaw.com/law-library/documents/fr%3A2015-02841. Public record. Not legal advice.