Clean Water Act Methods Update Rule for the Analysis of Effluent
Federal RegisterFeb 19, 2015
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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 <6 °C for a holding time of 28 days to prevent reduction of Cr(VI) to Cr(III). ASTM added an allowance for alternate holding times in Sections 1.3 and 9.2 if the user “demonstrates that holding time does not affect sample integrity per US EPA 40 CFR 136 . . .”
21. ASTM D 5673-10, dissolved elements and total-recoverable elements, ICP/MS; no substantive changes.
22. ASTM D 5907-13, filterable matter (total dissolved solids) and nonfilterable matter (total suspended solids), gravimetric, 180° gravimetric, 103-105° post washing of residue; no substantive changes.
23. ASTM D 6508-10, inorganic anions (fluoride, bromide, chloride, nitrite, nitrate, orthophosphate, and sulfate), capillary ion electrophoresis with indirect UV detection; no substantive changes.
24. ASTM D 7284-13, total cyanide, manual distillation with MgCl
2
followed by flow injection, gas diffusion amperometry; ASTM modified the method to include the use of a collector tube of the micro distillation apparatus with 1.5 ml of 1.0 M NaOH, and included information regarding the use of this collector tube in the procedure. ASTM also added information regarding the precision and bias associated with this method based on an interlaboratory study.
25. ASTM D 7511-12, total cyanide, segmented flow injection, in-line ultraviolet digestion, followed by gas diffusion amperometry; no substantive changes.
The following changes would apply to Table IC at 40 CFR part 136:
1. ASTM D 7065-11, nonylphenol, bisphenol A, p-tert-octylphenol, nonylphenol monoethoxylate, nonylphenol diethoxylate, gas chromatography/mass spectrometry (GC/MS); no substantive changes.
E. Changes to 40 CFR 136.3 To Include New United States Geological Survey (USGS) Methods
1. EPA proposes to add the USGS Methods I-2547-11 and I-2548-11 titled “Colorimetric Determination of Nitrate Plus Nitrite in Water by Enzymatic Reduction, Automated Discrete Analyzer Methods,” to Table IB for the analytes nitrate, nitrite, and combined nitrate-nitrite. Method I-2548-11 is a low level (analytical range) version of Method I-2547-11. They are both included in the same method title. The method can be found in USGS Survey Techniques and Methods, Book 5, Chapter B8. The method is available for free from the USGS Web site. This method follows the same procedure as in ATP Case No. N07-0003—Nitrate Elimination Company Inc.'s (NECi) Method N07-0003, Revision 9.0, March 2014, “Method for Nitrate Reductase Nitrate-Nitrogen Analysis,” which EPA also proposes to approve. Additional details on the ATP study and multi-laboratory validation can be found in Section E.1 below.
F. Changes to 40 CFR 136.3 to Include ATPs
To promote method innovation, EPA maintains a program that allows method developers to apply for EPA review of an alternative method to an existing approved method and potentially for EPA approval of that ATP. This ATP program is described for CWA applications at 40 CFR 136.4 and 136.5. EPA proposes for nationwide use six alternate test procedures. Based on EPA's review, the performance of these ATPs is equally effective as other methods already approved for measurement. These proposed new methods include: NECi Method N07-0003, “Method for Nitrate Reductase Nitrate-Nitrogen Analysis;” Timberline Instruments, LLC Method Ammonia-001, “Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis;” IDEXX Laboratories, Inc. Colilert®-18, “Coliform/
E. coli
Enzyme Substrate Test for fecal coliforms in Wastewater;” NCASI Method TNTP-W10900, “Total (Kjeldahl) Nitrogen and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion;” Hach Company Method 10242, “Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater;” and Hach Company Method 10206, “Spectrophotometric Measurement of Nitrate in Water and Wastewater.” Descriptions of these new methods included for approval are as follows:
1. The Nitrate Elimination Company Inc. (NECi) Method N07-0003, “Nitrate Reductase Nitrate-Nitrogen Analysis,” Revision 9.0, dated March 2014 (The Nitrate Elimination Company, Inc 2014a). The analysis measures nitrate, nitrite, and combined nitrate-nitrite. NECi Method N07-0003 is a “green” alternative to the other approved methods which use cadmium, a known carcinogen for the reduction of nitrate to nitrite prior to analyses. NECi Method N07-003 uses automated discreet analysis and spectrophotometry to determine concentrations of nitrate and nitrite, combined or separately in wastewater. The method involves the following steps:
• Enzymatic reduction of nitrate in a sample to nitrite using eukaryotic nitrate reductase;
• Diazotizing the nitrite originally in the sample plus the reduced nitrate with sulfanilamide followed by coupling with N-(1-napthyl)ethylenediamine dihydrochloride under acidic conditions to form a highly colored azo dye;
• Colorimetric determination in which the absorbance of color at 546 nm is directly proportional to the concentration of the nitrite plus the reduced nitrate in the sample;
• Measurement of nitrite separately, if needed, by analysis of the sample while eliminating the reduction step;
• Subtraction of the nitrite value from that of the combined nitrate-nitrite value to measure nitrate separately if needed.
NECi Method N07-0003 can be obtained from The Nitrate Elimination Company, 334 Hecla Street, Lake Linden, Michigan, 49945. Telephone: 906-370-1130.
2. Timberline Instruments, LLC Method Ammonia-001, “Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell Analysis,” dated June 24, 2011 (Timberline Instruments, LLC 2011a). Timberline Ammonia-001 is an automated method that uses a gas permeation cell and a conductivity detector to determine concentrations of ammonia in wastewater. The method involves the following steps:
• An aqueous sample is combined with sodium hydroxide to a pH above 11 producing ammonia in a non-ionized form in solution.
• This solution is conveyed to a membrane assembly and the gaseous ammonia in the aqueous sample migrates through the hydrophobic membrane into a borate buffer absorption solution, which is then transported to a conductivity cell.
• The measured changes in conductivity are used to quantitate ammonia in the sample using an external calibration.
Timberline Instruments, LLC Method Ammonia-001 can be obtained from Timberline Instruments, LLC, 1880 South Flatiron Court, Boulder, Colorado 80301. Telephone: 303-440-8779.
3. IDEXX Laboratories, Inc., Colilert®-18, “Coliform/
E. coli
Enzyme Substrate Test for fecal coliforms in Wastewater” (ATP Case No. N09-0004). The method is identical to the already approved
E. coli
Colilert®-18 method, with one exception. The current method was designed for total coliforms and
E. coli
, at an incubation temperature of 35 ± 0.5°C for these organisms. The addendum to the IDEXX Colilert®-18 method allows for incubation at 44.5 ± 0.2°C for fecal coliforms.
The Colilert®-18 Coliform/
E. coli
Enzyme Substrate Test can be obtained from IDEXX Laboratories Inc., One IDEXX Drive, Westbrook, ME 04092, Telephone: 1-800-321-0707.
4. National Council for Air and Stream Improvement, Inc. (NCASI) Method TNTP-W10900, “Total (Kjeldahl) Nitrogen (TKN) and Total Phosphorus in Pulp and Paper Biologically Treated Effluent by Alkaline Persulfate Digestion,” dated June 2011 (National Council for Air and Stream Improvement, Inc. 2011a). Unlike the other ATPs in the proposed rule, this method is for measurements in pulp, paper and paperboard mill biologically treated effluent only. NCASI Method TNTP-W10900 uses an alkaline persulfate digestion procedure to convert inorganic and organic nitrogen containing compounds to nitrate and inorganic and organic phosphorus containing compounds to orthophosphate which are then measured using a spectrophotometer to determine the concentration of total Kjeldahl nitrogen and total phosphorus in a sample.
The method involves the following steps:
• Oxidation of the inorganic and organic nitrogen containing compounds to nitrate and the inorganic and organic
forms of phosphorus to orthophosphate by heating acidified, unfiltered samples in the presence of persulfate (a strong oxidizer) at 120°C and 15 psi positive pressure for 30 minutes.
• Analysis of the digestate for measurement of nitrate and orthophosphate using the approved colorimetric procedures.
NCASI Method TNTP-W10900 can be obtained from The National Council for Air and Stream Improvement, Inc., Publications Coordinator, P.O. Box 13318, Research Triangle Park, NC 27709-3318, Telephone: 919-941-6400.
5. Hach Company Method 10242, “Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater,” Revision 1.1, dated January 10, 2013 (Hach Company 2013a). Hach Company Method 10242 is a simplified green chemistry alternative to the other approved methods for measuring TKN. The method uses less toxic reagents (
e.g.,
eliminating the use of mercuric sulfate). Hach Company Method 10242 uses a spectrophotometer to measure the concentration of total Kjeldahl nitrogen in a sample.
The method involves the following steps:
• Oxidation of the inorganic and organic nitrogen containing compounds to nitrate by digestion with peroxodisulfate;
• Reaction of nitrate with 2,6-dimethylphenol in a solution of sulfuric and phosphoric acid to form nitrodimethylphenol;
• Spectrophotometric measurement of the nitrodimethylphenol in which the absorbance of color at 345 nm is directly proportional to the concentration of total nitrogen in the sample;
• Measurement of oxidized forms of nitrogen (nitrite + nitrate) in the original sample in a second test vial;
• Subtraction of the concentration of the oxidized forms of nitrogen from the total nitrogen concentration resulting in the concentration of total Kjeldahl nitrogen in the sample.
Hach Company Method 10242 can be obtained from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539. Telephone: 970-669-3050.
6. Hach Company Method 10206, “Spectrophotometric Measurement of Nitrate in Water and Wastewater,” Revision 2.1, dated January 10, 2013 (Hach Company 2013b). Hach Company Method 1206 is a “green” alternative to the other approved methods which use cadmium, a known carcinogen for the reduction of nitrate to nitrite prior to analyses. Hach Company Method 10206 uses a spectrophotometer to measure the concentration of nitrate or combined nitrate-nitrite in a sample.
The method involves the following steps:
• Reaction of nitrate with 2,6-dimethylphenol in a solution of sulfuric and phosphoric acid to form nitrodimethylphenol;
• Spectrophotometric measurement of the nitrodimethylphenol in which the absorbance of color at 345 nm is directly proportional to the concentration of nitrate or, if the sample has been preserved with sulfuric acid, combined nitrate-nitrite in the sample.
Hach Company Method 10206 can be obtained from Hach Company, 5600 Lindbergh Drive, Loveland, CO 80539. Telephone: 970-669-3050.
G. Changes to 40 CFR part 136 to Align With 40 CFR part 122
The procedures approved in 40 CFR part 136 are often required as part of an application for a NPDES Permit NPDES, for reports required to be submitted under NPDES permits and/or for other requests for quantitative or qualitative effluent data under 40 CFR parts 122 and 125. EPA is clarifying the language in 40 CFR 136.1, 136.2, and 136.3 so that the term “Director” as used in 40 CFR part 136 parallels that in 40 CFR part 122. These sections use the terms “Administrator” and “State having an authorized program” and define these terms in 136.3. EPA proposes to revise these provisions to substitute the single term “Director” and define “Director” in section 40 CFR 136.3(d) by cross-reference to the definition of “Director” in the NPDES regulations at section 40 CFR 122.2.
EPA recently revised 40 CFR part 122 to include a definition of “sufficiently sensitive.” The term is used to describe what approved methods are adequate for NPDES permits. 40 CFR part 136.6(a)(2) uses the same term “sufficiently sensitive” in a different context to describe how sensitive a modified method should be compared to the original method. 40 CFR 136.6(a)(2) currently states that the modified method must be sufficiently sensitive and meet or exceed performance of the approved method(s) for the analyte(s) of interest, as documented by meeting the initial and ongoing quality control requirements in the method.
EPA proposes to delete the words “be sufficiently sensitive and” from 40 CFR 136.6(a)(2) to eliminate unnecessary confusion. It will not change the requirements of 40 CFR 136.6(a)(2). If a method modification meets or exceeds the performance of the approved method, this includes sensitivity.
H. Corrections to 40 CFR Part 136
These changes consist of typographical errors, updates that went unnoticed during the last update to 40 CFR part 136 to methods from VCSBs, and technology updates to toxicity methods.
1. EPA proposes to make a number of clarifications and corrections to its Whole Effluent Toxicity acute and chronic methods manuals (Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA-821-R-02-012, October 2002; Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA/821/R-02/013, October 2002; and Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA/821/R-02/014, October 2002) listed in Table IA. Clarifications include testing all concentrations rather than only high and low concentrations, definition of terms (
e.g.,
the acronym YCT—yeast, cereal leaves, and trout chow, is not defined), consistency corrections among the three manuals, notation that Cusum figure axes should be log scale, pH and temperature measurements should be done at the beginning of the test (rather than only at the end of the test), etc. Corrections also include deletion of unavailable products, typographical errors, etc.
2. EPA proposes to change the Standard Method listed for
E. coli
most probable number (MPN) in Tables IA and IH. During a previous revision, Standard Methods added sampling as section 9221B.1. As a result, section 9221B.1 in previously approved versions has become section 9221B.2. EPA proposes to change SM 9221B.1 to 9221B.2 in Tables IA and IH for
E. coli
MPN. The related footnotes in Tables IA and IH (12, 14 and 11, 13, respectively) are accurate and EPA does not propose to change them.
3. EPA proposes to change Table IA for Enterococci. EPA proposes to reinstate a line for Enterococci that was erroneously deleted in the 2012 Methods Update Rule. The line “MPN, multiple tube” with Standard Method 9230B-2007 should be added.
4. EPA proposes to change one of the Table IB hardness entries that currently states “Ca plus Mg as their carbonates, by inductively coupled plasma or AA direct aspiration. (See Parameters 13 and 33).” EPA proposes to revise the entry to “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.” The rationale behind this change is that if one calcium and magnesium method approved by EPA can be used to calculate hardness, then other approved EPA methods should also be permitted to do so.
5. EPA proposes to edit Table IB, footnote 24. EPA proposes to delete “p 14” from the footnote because the method is not on that page.
6. EPA proposes to delete Method 200.5, in Table IB from the cobalt, molybdenum and thallium entries. These analytes have not undergone formal testing by this method, and this method should not have been approved for these analytes.
7. EPA proposes to remove the reference to costs in 40 CFR 136.3 because costs are not included in the referenced documents.
8. EPA proposes to remove the first instance of “are” in 40 CFR 136.3(e) because it is an error.
I. Changes to Table II at 40 CFR 136.3(e) to Required Containers, Preservation Techniques, and Holding Times
EPA proposes revisions to Table II at 40 CFR 136.3(e) to amend some of the current requirements.
1. EPA proposes to add rows to Table II that specify holding times for total/fecal coliforms, and fecal streptococci in Table IH. Currently these bacterial tests are unspecified. EPA proposes the same holding time requirements as the other bacterial tests.
2. EPA proposes to change the sodium thiosulfate concentrations in Table II for bacterial tests from 0.0008% sodium thiosulfate to 0.008%. EPA proposed this change in its last update to 40 CFR part 136 (75 FR 58066-58067), but inadvertently omitted it in the publication of the final rule.
3. EPA proposes to re-insert language that was accidentally deleted from footnote 5 of Table II during the last update to 40 CFR part 136. Footnote 5 currently reads “ASTM D7365-09a specifies treatment options for samples containing oxidants (
e.g.,
chlorine). Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses dechlorination procedures.” EPA proposes to revise the footnote to read “ASTM D7365-09a specifies treatment options for samples containing oxidants (
e.g.,
chlorine) for cyanide analysis. Also, Section 9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses dechlorination procedures for microbiological analyses.” The footnote needs to specify that treatment options for samples containing oxidants is specifically for cyanide analysis, and that the dechlorination procedures are specifically for microbiological analyses.
4. EPA seeks comment on how to approve variances to sample preservation, containers or holding times listed in Table II for specific dischargers. Before the 2012 Final Method Update Rule (FR 77: 29758), the regulation required parties requesting a variance from Table II for specific dischargers to send the request to the appropriate EPA regional office for review, and then for the regional office to send the request to the National ATP Coordinator at EPA Headquarters for review and recommendation. Following receipt of such recommendation, the regional office could approve a variance. In the 2012 Final Method Update Rule, EPA changed the requirement so that either the Regional ATP Coordinator or the permitting authority could approve an exception to Table II for specific dischargers. The primary rationale for this change, as stated in the preamble of the 2010 Proposed Method Update Rule (FR 76: 77742) was: “EPA is revising the text at 136.3(e) to allow a party to explain, without a cumbersome waiver process, to their permitting or other authority their basis for an alternative approach.” Giving this authority to either the Regional ATP Coordinator or the permitting authority speeds up the approval process. Also, the permitting authority is more likely to know about special circumstances surrounding the local dischargers (
e.g.,
unusual discharge matrices, remote locations, etc.).
This change in the approval process resulted in the following potential complications and EPA is interested in public comment on them. First, it created a parallel authority to approve variances to Table II for specific dischargers. A discharger could make a request to both the Regional ATP Coordinator and the permitting authority, receive contradictory answers, and then choose the answer that the discharger prefers. Second, when there are different authorities approving a Table II variance for specific dischargers, there is potential for the data and documentation required by one authority to differ significantly from that required by the other authority.
EPA seeks comment on potential paths forward that would eliminate these concerns, while streamlining the process so that approval can be granted within the EPA region or by the state permitting authority. One possibility is for the permitting authority and the Regional ATP Coordinator to approve Table II variances for specific dischargers collaboratively. The permitting authority could provide the initial review and approval, and then approved requests could be sent to the Regional ATP Coordinator for final review and approval. Both organizations would need to agree for specific dischargers to be allowed Table II variances. Another option is to give the Regional ATP Coordinator exclusive rights to approve Table II variances for specific dischargers. Another option is to give the permitting authority exclusive rights to approve Table II variances. Other options are also possible, such as leaving 40 CFR 136.3(e) unchanged.
EPA also seeks comment on what data should be submitted to support a request for a Table II variance for a specific discharger. 40 CFR 136.3(e) requires that data be included with any request to modify Table II requirements for a specific discharger. The data would need to prove that the variance does not compromise the analytical results.
J. Clarifications/Corrections to ATP Procedures in 40 CFR 136.4, 136.5 and Allowed Modifications in 136.6
40 CFR 136.4 and 136.5 describe EPA procedures for obtaining approval to use an alternate test procedures either on a national basis, or for limited use by dischargers or facilities specified in the approval. In the 2012 Method Update Rule, EPA made several clarifying changes to the language of these sections. At the same time, however, in many places in 40 CFR 136.4 and 136.5 where the phrase “Regional Alternate Test Procedures Coordinator” or “Regional ATP Coordinator” appears, EPA inadvertently also inserted the phrase “or permitting authority” following the phrase. This error resulted from the use of the “search and replace” function on the computer. The effect of the change was to inadvertently authorize
State
permitting authorities to approve ATPs for limited use within the State. EPA never intended this result as is demonstrated by two facts. First, in its proposal for the 2012 Update, EPA did not propose to authorize State NPDES permitting authorities to approve limited use ATPs. Second, the rule states that the approval may be restricted to specific dischargers or facilities, or to all dischargers or facilities “specified in the approval
for the Region.”
(emphasis added). This language evidences EPA's intent that the Region—not the state—would be
authorized to issue any such limited use ATP approval. Finally, as further evidence of EPA's intent, in several places, the text of the rule makes more sense if read to authorize only the Regional ATP Coordinator, and not the State permitting authority, to approve limited use ATPs. For example, 40 CFR 136.5(d)(1) provides that after a review of the application by the Alternate Test Procedure Regional ATP Coordinator or permitting authority, the Regional ATP Coordinator or permitting authority notifies the applicant and the appropriate State agency of approval or rejection of the use of the alternate test procedure.
As currently written, if the State is acting on a request for approval, the regulation would require the State to inform itself of its own action in approving or rejecting the ATP, a somewhat superfluous requirement.
Consequently, EPA proposes to delete all instances of “or permitting authority” from 40 CFR 136.4 and 136.5 to correct this error and revise the rule text to its original intent. Based on this revision, EPA and EPA alone would have the authority to approve limited use ATPs.
EPA also proposes changes to 40 CFR 136.4 and 136.5 to clarify the process for nationwide approval and the Regional ATP Coordinator's role in limited use ATP approvals. These changes do not significantly change the process, the intent is to make wording simpler and clearer.
Finally, EPA proposes to add language to 40 CFR 136.6(b)(1) to clarify that if a method user is uncertain whether or not a modification is allowed under 40 CFR 136.6, the user should contact either its Director or EPA Regional ATP Coordinator.
K. Changes to Appendix B to 40 CFR part 136—Definition and Procedure for the Determination of the MDL
EPA proposes revisions to the procedure for determination of the MDL primarily to address laboratory blank contamination and to better account for intra-laboratory variability. EPA's consideration of revisions to the MDL procedure for this rulemaking is specific to these revisions, and other changes to the procedure are outside the scope of this action. The proposed changes originated from The National Environmental Laboratory Accreditation Conference Institute and also reflect review by EPA, states, and commercial laboratories. The proposed revisions address the following issues and would add new requirements.
Background contamination: laboratories would be required to evaluate the MDL to account for background levels of contamination. As laboratory methods become more and more sensitive, background levels of contamination are more likely to contribute to the result. This modification would reduce false positive detects.
MDLs that represent multiple instruments: if a laboratory uses MDL values that represent multiple instruments, then the laboratory would be required to calculate the MDL using spiked samples and blank samples from all of these instruments. Currently, laboratories can run all of their MDL samples on the most sensitive instrument, and then use that MDL for other instruments. This modification will make the MDL more representative of the laboratory's actual capability.
Ongoing MDL quarterly verification: laboratories would be required to check their MDL values once a quarter. Currently, laboratories can run MDL samples once a year under the most ideal circumstances (
e.g.,
immediately after the instrument has been serviced or after an annual maintenance routine). Quarterly evaluation will determine if the detection limit has significantly drifted during the year. Laboratories would be exempt from running these samples for a method during quarters when no samples are run using that method.
EPA requests comment on whether it should adopt these proposed changes, in part, or in whole.
V. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review and Review and Executive Order 13563: Improving Regulation and Regulatory Review
This rule is not a significant regulatory action and was therefore not submitted to the Office of Management and Budget for review.
B. Paperwork Reduction Act
This action does not impose an information collection burden under the PRA. This rule does not impose any information collection, reporting, or recordkeeping requirements. This proposal would merely add or revise CWA test procedures.
C. Regulatory Flexibility Act
I certify that this action would not have a significant economic impact on a substantial number of small entities under the RFA. This action will not impose any requirements on small entities. This action would approve new and revised versions of CWA testing procedures. Generally, these changes would have a positive impact on small entities by increasing method flexibility, thereby allowing entities to reduce costs by choosing more cost-effective methods. In general, EPA expects the proposed revisions would lead to few, if any, increased costs. As explained previously, most of the proposed changes clarify procedures for EPA approval of ATPs, clarify or improve the instructions in the method, update the technology used in the method, improve the QC instructions, make editorial corrections, or reflect the most recent approval year of an already approved method. In some cases, the proposal would add alternatives to currently approved methods for a particular analyte (
e.g.
Method N07-0003 for Nitrate Reductase Nitrate-Nitrogen Analysis). Because these methods would be alternatives rather than requirements, there are no direct costs associated with their proposal. EPA proposes methods that would be incorporated by reference. If a permittee elected to use these methods, they could incur a small cost associated with obtaining these methods. See Section IV.B. Finally, the proposed changes to the MDL procedure would lead to limited increased costs. In the vast majority of cases, laboratories already collect samples that could be used in the revised procedure and/or would simply adjust the time period of collection. The total number of MDL samples run annually would only increase to any appreciable extent for laboratories that own many instruments. EPA has not estimated costs for these cases, because such costs, if incurred, would be negligible in comparison to overall laboratory expenditures.
D. Unfunded Mandates Reform Act
This action does not contain any unfunded mandate as described in UMRA, 2 U.S.C. 1531-1538, and does not significantly or uniquely affect small governments. The action imposes no enforceable duty on any state, local or tribal governments or the private sector.
E. Executive Order 13132: Federalism
This proposed rule does not have federalism implications. It will not have substantial direct effects on the states, on the relationship between the national government and the states, or on the distribution of power and responsibilities among the various levels of government.
F. Executive Order 13175: Consultation and Coordination with Indian Tribal Governments
This proposed rule does not have tribal implications as specified in Executive Order 13175. This rule would merely approve new and revised versions of test procedures. EPA does not expect the proposal would lead to any costs to any tribal governments, and if incurred, projects they would be minimal. Thus, Executive Order 13175 does not apply to this action.
G. Executive Order 13045: Protection of Children from Environmental Health Risks and Safety Risks
EPA interprets EO 13045 as applying only to those regulatory actions that concern environmental health or safety risks that the EPA has reason to believe may disproportionately affect children, per the definition of “covered regulatory action” in section 2-202 of the Executive Order. This action is not subject to Executive Order 13045 because it does not concern an environmental health risk or safety risk.
H. Executive Order 13211: Actions that Significantly Affect Energy Supply, Distribution, or Use
This action is not subject to Executive Order 13211 because it is not a significant regulatory action under Executive Order 12866.
I. National Technology Transfer and Advancement Act of 1995
This action involved technical standards. The EPA proposes to approve the use of technical standards developed and recommended by the Standard Methods Committee and ASTM International for use in compliance monitoring where EPA determined that those standards meet the needs of CWA programs. As explained in Section IV.C, EPA does not propose to add one SM method because it did not receive data to demonstrate that the method had undergone full inter-laboratory validation. EPA proposes all other methods recommended by VCSBs in advance of the proposed rule.
J. Executive Order 12898: Federal Actions To Address Environmental Justice in Minority Populations and Low-Income Populations
The EPA believes the human health or environmental risk addressed by this action will not have potential disproportionately high and adverse human health or environmental effects on minority, low-income or indigenous populations.
List of Subjects in 40 CFR Part 136
Environmental protection, Incorporation by reference, Reporting and recordkeeping requirements, Test procedures, Water pollution control.
Dated: February 5, 2015.
Gina McCarthy,
Administrator.
For the reasons set out in the preamble, title 40, chapter I of the Code of Federal Regulations is proposed to be amended as follows:
PART 136—GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS
1. The authority citation for part 136 continues to read as follows:
Authority:
Secs. 301, 304(h), 307 and 501(a), Pub. L. 95-217, 91 Stat. 1566,
et seq.
(33 U.S.C. 1251,
et seq.
) (the Federal Water Pollution Control Act Amendments of 1972 as amended by the Clean Water Act of 1977).
2. Section 136.1 is amended by revising paragraph (a) to read as follows:
§ 136.1
Applicability.
(a) The procedures prescribed herein shall, except as noted in §§ 136.4, 136.5, and 136.6, be used to perform the measurements indicated whenever the waste constituent specified is required to be measured for:
(1) An application submitted to the Director and/or reports required to be submitted under NPDES permits or other requests for quantitative or qualitative effluent data under parts 122 to 125 of this chapter; and
(2) Reports required to be submitted by dischargers under the NPDES established by parts 124 and 125 of this chapter; and
(3) Certifications issued by States pursuant to section 401 of the Clean Water Act (CWA), as amended.
3. Section 136.2 is amended by revising paragraph (d) to read as follows:
§ 136.2
Definitions.
(d)
Director
means the director as defined in 40 CFR 122.2.
4. In § 136.3:
a. Revise paragraph (a) introductory text and tables IA, IB, IC, ID, IF, IG, and IH.
b. Revise paragraphs (b) introductory text, (b)(8)(iv), (b)(8)(v), (b)(8)(xiii), (b)(8)(xv), (b)(10)(viii), (b)(10)(x) through (lviii), (b)(10)(lxi) through (lxiii), (b)(10)(lxviii), (b)(15)(v), (b)(15)(viii) through (x), (b)(15)(xii), (b)(15)(xiii), (b)(15)(xv) through (xvii), (b)(15)(xxii) through (xxiv), (b)(15)(xxx), (b)(15)(xxxv), (b)(15)(xxxvii), (b)(15)(xxxix), (b)(15)(xlii), (b)(15)(l), (b)(15)(lii), (b)(15)(lv), (b)(15)(lviii), (b)(15)(lxi), (b)(15)(lxvi), and (b)(15)(lxviii).
c. Redesignate paragraphs (b)(19)(vii) and (viii) as paragraphs (b)(19)(ix) and (x), respectively.
d. Add paragraphs (b)(19)(vii) and (viii).
e. Revise paragraphs (b)(20)(i) through (iv).
f. Remove paragraph (b)(20)(v).
g. Revise paragraph (b)(25).
h. Redesignate paragraphs (b)(33) and (34) as paragraphs (b)(35) and (36), respectively, and redesignate paragraphs (b)(26) through (32) as paragraphs (b)(27) through (33), respectively.
i. Add paragraph (b)(26).
j. Add paragraph (b)(34).
k. Revise newly redesignated paragraph (b)(35).
l. Revise paragraph (c) and the table in paragraph (e).
The revisions and additions read as follows:
§ 136.3
Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are listed together with test procedure descriptions and references in Tables IA, IB, IC, ID, IE, IF, IG, and IH of this section. The methods listed in Tables IA, IB, IC, ID, IE, IF, IG, and IH are incorporated by reference, see paragraph (b) of this section, with the exception of EPA Methods 200.7, 601-613, 624.1, 625.1, 1613, 1624, and 1625. The full texts of Methods 601-613, 624.1, 625.1, 1613, 1624, and 1625 are printed in appendix A of this part, and the full text of Method 200.7 is printed in appendix C of this part. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part. In the event of a conflict between the reporting requirements of 40 CFR parts 122 and 125 and any reporting requirements associated with the methods listed in these tables, the provisions of 40 CFR parts 122 and 125 are controlling and will determine a permittee's reporting requirements. The full text of the referenced test procedures are incorporated by reference into Tables IA, IB, IC, ID, IE, IF, IG, and IH. The date after the method number indicates the latest editorial change of the method. The discharge parameter values for which reports are required must be determined by one of the standard analytical test procedures incorporated by reference and described in Tables IA,
IB, IC, ID, IE, IF, IG, and IH or by any alternate test procedure which has been approved by the Administrator under the provisions of paragraph (d) of this section and §§ 136.4 and 136.5. Under certain circumstances paragraph (c) of this section, § 136.5(a) through (d) or 40 CFR 401.13, other additional or alternate test procedures may be used.
Table IA—List of Approved Biological Methods for Wastewater and Sewage Sludge
Parameter and units
Method
1
EPA
Standard methods
AOAC, ASTM, USGS
Other
Bacteria:
1. Coliform (fecal), number per 100 mL or number per gram dry weight
Most Probable Number (MPN), 5 tube, 3 dilution, or
p. 132
3
1680
11 15
1681
11 20
9221 C E-2006
Multiple tube/multiple well, or
Colilert-18 ®
13 18 29
Membrane filter (MF)
2
, single step
p. 124
3
9222 D-2006
30
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
30
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
5
p. 111
3
9222 B−2006
5.
E. coli,
number per 100 mL
21
MPN
6 8 16
multiple tube, or
9221B.2-2006/9221F-2006
12 14
multiple tube/multiple well, or
9223 B-2004
13
991.15
10
Colilert®
13 18
Colilert-18®
13 17 18
MF
2 6 7 8
single step
1603
22
mColiBlue-24 ®
19
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
21
MPN, 5 tube, 3 dilution, or
p. 139
3
9230 B-2007
MPN
6 8
, multiple tube/multiple well, or
9230 D-2007
D6503-99
9
Enterolert ®
13 24
MF
2 6 7 8
single step or
1600
25
9230 C-2007
Plate count
p. 143
3
8.
Salmonella
, number per gram dry weight
11
MPN multiple tube
1682
23
Aquatic Toxicity:
9. Toxicity, acute, fresh water organisms, LC
50
, percent effluent
Ceriodaphnia dubia
acute
2002.0
26
Daphnia puplex
and
Daphnia magna
acute
2021.0
26
Fathead Minnow,
Pimephales promelas,
and Bannerfin shiner,
Cyprinella leedsi,
acute
2000.0
26
Rainbow Trout,
Oncorhynchus mykiss,
and brook trout,
Salvelinus fontinalis,
acute
2019.0
26
10. Toxicity, acute, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, LC
50
, percent effluent
Mysid,
Mysidopsis bahia,
acute
2007.0
26
Sheepshead Minnow,
Cyprinodon variegatus,
acute
2004.0
26
Silverside,
Menidia beryllina, Menidia menidia,
and
Menidia peninsulae,
acute
2006.0
26
11. Toxicity, chronic, fresh water organisms, NOEC or IC
25
, percent effluent
Fathead minnow,
Pimephales promelas,
larval survival and growth
1000.0
27
Fathead minnow,
Pimephales promelas,
embryo-larval survival and teratogenicity
1001.0
27
Daphnia,
Ceriodaphnia dubia,
survival and reproduction
1002.0
27
Green alga,
Selenastrum capricornutum,
growth
1003.0
27
12. Toxicity, chronic, estuarine and marine organisms of the Atlantic Ocean and Gulf of Mexico, NOEC or IC
25
, percent effluent
Sheepshead minnow,
Cyprinodon variegatus,
larval survival and growth
1004.0
28
Sheepshead minnow,
Cyprinodon variegatus,
embryo-larval survival and teratogenicity
1005.0
28
Inland silverside,
Menidia beryllina,
larval survival and growth
1006.0
28
Mysid,
Mysidopsis bahia,
survival, growth, and fecundity
1007.0
28
Sea urchin,
Arbacia punctulata,
fertilization
1008.0
28
Table IA 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 been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.
8
To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.
9
Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.
10
Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.
11
Recommended for enumeration of target organism in sewage sludge.
12
The multiple-tube fermentation test is used in 9221B.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.
13
These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme β-glucuronidase produced by
E. coli.
14
After prior enrichment in a presumptive medium for total coliform using 9221B.2-2006, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F-2006. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 µg/mL of MUG may be used.
15
Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-14-009. September 2014. U.S. EPA.
16
Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray® and the MPN calculated from the table provided by the manufacturer.
17
Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and
E. coli
that provides results within 18 h of incubation at 35°C rather than the 24 h required for the Colilert® test and is recommended for marine water samples.
18
Descriptions of the Colilert®, Colilert-18®, and Quanti-Tray® may be obtained from IDEXX Laboratories, Inc.
19
A description of the mColiBlue24® test, is available from Hach Company.
20
Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.
21
Recommended for enumeration of target organism in wastewater effluent.
22
Method 1603:
Escherichia coli
(
E. coli
) in Water by Membrane Filtration Using Modified membrane-Thermotolerant
Escherichia coli
Agar (modified mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.
23
Method 1682:
Salmonella
in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. July 2014. U.S. EPA.
24
A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc.
25
Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-β-D-Glucoside Agar (mEI), EPA-821-R-14-011. September 2014. U.S. EPA.
26
Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms, EPA-821-R-02-012. Fifth Edition, October 2002. U.S. EPA.
27
Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms, EPA-821-R-02-013. Fourth Edition, October 2002. U.S. EPA.
28
Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms, EPA-821-R-02-014. Third Edition, October 2002. U.S. EPA.
29
Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and
E. coli
that has been adapted to detect fecal coliforms. To use Colilert-18® to assay for fecal coliforms, the incubation temperature is 44.5
+
0.2°C. This test is recommended for wastewater samples.
30
The verification frequency is at least five typical and five atypical colonies per sampling site on the day of sample collection and analysis.
Table IB—List of Approved Inorganic Test Procedures
Parameter
Methodology
58
EPA
52
Standard methods
ASTM
USGS/AOAC/Other
1. Acidity, as CaCO
3
, mg/L
Electrometric endpoint or phenolphthalein endpoint
2310 B-2011
D1067-11
I-1020-85.
2
2. Alkalinity, as CaCO
3
, mg/L
Electrometric or Colorimetric titration to pH 4.5, Manual
2320 B-1997
D1067-11
973.43
3
, I-1030-85.
2
Automatic
310.2 (Rev. 1974)
1
I-2030-85.
2
3. Aluminum—Total,
4
mg/L
Digestion
4
, followed by any of the following:
AA direct aspiration
36
3111 D-2011 or 3111 E-2011
I-3051-85.
2
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
Direct Current Plasma (DCP)
36
D4190-08
See footnote.
34
Colorimetric (Eriochrome cyanine R)
3500-Al B-2011
4. Ammonia (as N), mg/L
Manual distillation
6
or gas diffusion (pH > 11), followed by any of the following:
350.1, Rev. 2.0 (1993)
4500-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 < 20% RPD for all tested matrices). Alternatively the two populations of spike recovery percentages may be compared using a recognized statistical test.
7
Industrial Method Number 379-75 WE Ammonia, Automated Electrode Method, Technicon Auto Analyzer II. February 19, 1976. Bran & Luebbe Analyzing Technologies Inc.
8
The approved method is that cited in Methods for Determination of Inorganic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1. 1979. USGS.
9
American National Standard on Photographic Processing Effluents. April 2, 1975. American National Standards Institute.
10
In-Situ Method 1003-8-2009, Biochemical Oxygen Demand (BOD) Measurement by Optical Probe. 2009. In-Situ Incorporated.
11
The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
12
Carbonaceous biochemical oxygen demand (CBOD
5
) must not be confused with the traditional BOD
5
test method which measures “total BOD.” The addition of the nitrification inhibitor is not a procedural option, but must be included to report the CBOD
5
parameter. A discharger whose permit requires reporting the traditional BOD
5
may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's permit specifically states CBOD
5
is required can the permittee report data using a nitrification inhibitor.
13
OIC Chemical Oxygen Demand Method. 1978. Oceanography International Corporation.
14
Method 8000, Chemical Oxygen Demand, Hach Handbook of Water Analysis, 1979. Hach Company.
15
The back titration method will be used to resolve controversy.
16
Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70. 1977. Orion Research Incorporated. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing 0.2, 1.0, and 5.0 mL 0.00281 N potassium iodate/100 mL solution, respectively.
17
Method 245.7, Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA-821-R-05-001. Revision 2.0, February 2005. US EPA.
18
National Council of the Paper Industry for Air and Stream Improvement (NCASI) Technical Bulletin 803, May 2000.
19
Method 8506, Biocinchoninate Method for Copper, Hach Handbook of Water Analysis. 1979. Hach Company.
20
When using a method with block digestion, this treatment is not required.
21
Industrial Method Number 378-75WA, Hydrogen ion (pH) Automated Electrode Method, Bran & Luebbe (Technicon) Autoanalyzer II. October 1976. Bran & Luebbe Analyzing Technologies.
22
Method 8008, 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water. 1980. Hach Company.
23
Method 8034, Periodate Oxidation Method for Manganese, Hach Handbook of Wastewater Analysis. 1979. Hach Company.
24
Methods for Analysis of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3, (1972 Revised 1987). 1987. USGS.
25
Method 8507, Nitrogen, Nitrite-Low Range, Diazotization Method for Water and Wastewater. 1979. Hach Company.
26
Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
27
The colorimetric reaction must be conducted at a pH of 10.0 ± 0.2.
28
Addison, R.F., and R.G. Ackman. 1970. Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,
Journal of Chromatograph
y, 47(3):421-426.
29
Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be diluted to 100 mL by adding 40 mL each of 2 M Na
2
S
2
O
3
and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the approved method is satisfactory.
30
The use of EDTA decreases method sensitivity. Analysts may omit EDTA or replace with another suitable complexing reagent provided that all method specified quality control acceptance criteria are met.
31
For samples known or suspected to contain high levels of silver (
e.g.,
in excess of 4 mg/L), cyanogen iodide should be used to keep the silver in solution for analysis. Prepare a cyanogen iodide solution by adding 4.0 mL of concentrated NH
4
OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I
2
to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH>7 with 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; Se
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