Document ID: EPA-HQ-OW-2022-0901-0001
Agency: epa
Document Type: Proposed Rule
Title: Clean Water Act Methods Update Rule for the Analysis of Effluent
Posted Date: 2023-02-21T05:00Z

[Federal Register Volume 88, Number 34 (Tuesday, February 21, 2023)]
[Proposed Rules]
[Pages 10724-10771]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2023-02391]

[[Page 10723]]

Vol. 88

Tuesday,

No. 34

February 21, 2023

Part III

Environmental Protection Agency

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40 CFR Part 136

Clean Water Act Methods Update Rule for the Analysis of Effluent; 
Proposed Rule

  Federal Register / Vol. 88, No. 34 / Tuesday, February 21, 2023 / 
Proposed Rules  

[[Page 10724]]

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 136

[EPA-HQ-OW-2022-0901; FRL-9346-01-OW]
RIN 2040-AG25

Clean Water Act Methods Update Rule for the Analysis of Effluent

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: The Environmental Protection Agency (EPA) is proposing changes 
to its test procedures required to be used by industries and 
municipalities when analyzing the chemical, physical, and biological 
properties of wastewater and other samples for reporting under EPA's 
National Pollutant Discharge Elimination System (NPDES) permit program. 
The Clean Water Act (CWA) requires EPA to promulgate these test 
procedures (analytical methods) for analysis of pollutants. EPA 
anticipates that these proposed changes would provide increased 
flexibility for the regulated community in meeting monitoring 
requirements while improving data quality. In addition, this proposed 
update to the CWA methods would incorporate technological advances in 
analytical technology and make a series of minor changes and 
corrections to existing approved methods. As such, EPA expects that 
there would be no negative economic impacts resulting from these 
proposed changes.

DATES: Comments on this proposed rule must be received on or before 
April 24, 2023.

ADDRESSES: You may send comments, identified by Docket ID No. EPA-HQ-
OW-2022-0901 by any of the following methods:
     Federal eRulemaking Portal: https://www.regulations.gov 
(our preferred method). Follow the online instructions for submitting 
comments.
     Email: [email protected]. Include Docket ID No. EPA-HQ-OW-
2022-0901 in the subject line of the message.
     Mail: U.S. Environmental Protection Agency, EPA Docket 
Center, Office of Water Docket, Mail Code 28221T, 1200 Pennsylvania 
Avenue NW, Washington, DC 20460.
     Hand Delivery or Courier: EPA Docket Center, WJC West 
Building, Room 3334, 1301 Constitution Avenue NW, Washington, DC 20004. 
The Docket Center's hours of operations are 8:30 a.m.-4:30 p.m., 
Monday-Friday (except Federal Holidays).
    Instructions: All submissions received must include the Docket ID 
No. for this rulemaking. Comments received may be posted without change 
to https://www.regulations.gov/, including any personal information 
provided. For detailed instructions on sending comments and additional 
information on the rulemaking process, see the ``Public Participation'' 
heading of the SUPPLEMENTARY INFORMATION section of this document.

FOR FURTHER INFORMATION CONTACT: Tracy Bone, Engineering and Analysis 
Division (4303T), Office of Water, Environmental Protection Agency, 
1200 Pennsylvania Avenue NW, Washington, DC 20460-0001; telephone 
number: 202-564-5257; email address: [email protected].

SUPPLEMENTARY INFORMATION: 

Table of Contents

I. Public Participation
II. General Information
III. Background
IV. Incorporation by Reference
V. Statutory and Executive order Reviews

I. Public Participation

A. Written Comments

    Submit your comments, identified by Docket ID No. EPA-HQ-OW-2022-
0901, at https://www.regulations.gov (our preferred method), or the 
other methods identified in the ADDRESSES section. Once submitted, 
comments cannot be edited or removed from the docket. EPA may publish 
any comment received to its public docket. Do not submit to EPA's 
docket at https://www.regulations.gov any information you consider to 
be Confidential Business Information (CBI), Proprietary Business 
Information (PBI), or other information whose disclosure is restricted 
by statute. Multimedia submissions (audio, video, etc.) must be 
accompanied by a written comment. The written comment is considered the 
official comment and should include discussion of all points you wish 
to make. EPA will generally not consider comments or comment contents 
located outside of the primary submission (i.e., on the web, cloud, or 
other file sharing system). Please visit https://www.epa.gov/dockets/commenting-epa-dockets for additional submission methods; the full EPA 
public comment policy; information about CBI, PBI, or multimedia 
submissions; and general guidance on making effective comments. 
Publicly available docket materials are available electronically in 
www.regulations.gov at the Water Docket in EPA Docket Center, EPA/DC, 
EPA West William J. Clinton Building, Room 3334, 1301 Constitution 
Avenue NW, Washington, DC. The Public Reading Room is open from 8:30 
a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. Any 
copyright material can be viewed at the Reading Room, please contact 
the EPA Docket Center, public Reading Room. The telephone number for 
the Public Reading Room is 202-566-1744, and the telephone number for 
the Water Docket is 202-566-2426. Fax: 202-566-9744. Email: [email protected].

II. General Information

A. Does this action apply to me?

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

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                  Category                                 Examples of potentially affected entities
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State, Territorial, and Indian Tribal         States authorized to administer the National Pollutant Discharge
 Governments.                                  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; the environmental monitoring industry.
Municipalities..............................  Publicly Owned Treatment Works (POTWs) or other municipality-owned
                                               facilities that must conduct monitoring to comply with NPDES
                                               permits.
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    This table is not intended to be exhaustive, but rather provides a 
guide for readers regarding entities likely to be affected by this 
action. This table lists types of entities that 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

[[Page 10725]]

and applicability). If you have questions regarding the applicability 
of this action to a particular entity, consult the appropriate person 
listed in the preceding FOR FURTHER INFORMATION CONTACT section.

B. What action is the Agency taking?

    Periodically, EPA proposes to update the approved methods in 40 CFR 
part 136. In general, the changes proposed in this action fall into the 
following categories. The first category is updated versions of EPA 
methods currently approved in 40 CFR part 136. The second category is 
new or revised methods published by a voluntary consensus standard body 
(VCSB) or the United States Geologic Survey (USGS) that are similar to 
methods previously adopted as EPA-approved methods in 40 CFR part 136. 
The third category is methods EPA has reviewed under the agency's 
national Alternate Test Procedure (ATP) program and preliminarily 
concluded are appropriate for nationwide use. Finally, EPA is proposing 
certain corrections or amendments to the text and tables of 40 CFR part 
136. EPA is proposing adoption of these revisions to improve data 
quality, update methods to keep current with technology advances, and 
provide the regulated community with greater flexibility. The following 
paragraphs provide details on the proposed revisions.

C. What is the agency's authority for taking this action?

    EPA is proposing this regulation under the authorities of sections 
301(a), 304(h), and 501(a) of the CWA; 33 U.S.C. 1251, 1311(a), 1314(h) 
and 1361(a). Section 301(a) of the CWA prohibits the discharge of any 
pollutant into navigable waters unless the discharge complies with, 
among other provisions, an NPDES permit issued under section 402 of the 
CWA. Section 304(h) of the CWA requires EPA Administrator to ``. . . 
promulgate guidelines establishing test procedures for the analysis of 
pollutants that shall include the factors which must be provided in any 
certification pursuant to [section 401 of the CWA] or permit 
application pursuant to [section 402 of the CWA].'' Section 501(a) of 
the CWA authorizes the 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).

III. Background

    This preamble describes the abbreviations and acronyms; reasons for 
the proposed rule; and a summary of the proposed changes and 
clarifications; the legal authority for the proposed rule; methods 
incorporated by reference; a summary of the proposed changes and 
clarifications and solicits comment from the public.

Abbreviations and Acronyms Used in the Preamble and Proposed Rule Text

ADMI: American Dye Manufacturers Institute
ASTM: ASTM International \1\
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    \1\ Formerly known as the American Society for Testing and 
Materials (ASTM).
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ATP: Alternate Test Procedure
BHI: Brain heart infusion
BOD5: 5-day Biochemical Oxygen Demand
CATC: Cyanide Amenable to Chlorination
CBI: Confidential Business Information
CFR: Code of Federal Regulations
CIE: Capillary Ion Electrophoresis
CNCl: Cyanogen Chloride
CWA: Clean Water Act
EC-MUG: EC broth with 4-methylumbelliferyl-[beta]-D-glucuronide
EDTA: Ethylenediaminetetraacetic acid
EPA: Environmental Protection Agency
DO: Dissolved Oxygen
GC: Gas Chromatography
GC/MS/MS: Gas Chromatography-Tandem Mass Spectrometry
GC/HRMS: Gas Chromatography-High Resolution Mass Spectrometry
ICP/AES: Inductively Coupled Plasma-Atomic Emission Spectroscopy
MIBK: Methyl Isobutyl Ketone
NED: N-(1-naphthyl)-ethylenediamine dihydrochloride
MF: Membrane Filtration
MgCl2: Magnesium Chloride
MPN: Most Probable Number
nm: Nanometer
NPDES: National Pollutant Discharge Elimination System
NTTAA: National Technology Transfer and Advancement Act
QC: Quality Control
STGFAA: Stabilized Temperature Graphite Furnace Atomic Absorption 
Spectroscopy
TKN: Total Kjeldahl Nitrogen
TOC: Total Organic Carbon
USGS: United States Geological Survey
VCSB: Voluntary Consensus Standards Body

    NPDES 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 method.\2\
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    \2\ NPDES permit regulations also specify that the approved 
method needs to be sufficiently sensitive. See 40 CFR 122.21(e)(3).
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    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-approved analytical methods must be used 
include the following: (1) applications for NPDES permits, (2) sampling 
or other reports required under NPDES permits, (3) other requests for 
quantitative or qualitative effluent data under the NPDES regulations, 
(4) State CWA 401 certifications, and (5) sampling and analysis 
required under EPA's General Pretreatment Regulations for Existing and 
New Sources of Pollution, 40 CFR 136.1 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 proposed in this action fall into the 
following categories. The first category is updated versions of EPA 
methods currently approved in 40 CFR part 136. The second is new or 
revised methods published by the VCSBs or the USGS that are similar to 
methods previously adopted as EPA-approved methods in 40 CFR part 136. 
The third category is methods EPA has reviewed under the Agency's 
national ATP program and preliminarily concluded are appropriate for 
nationwide use. Finally, EPA is proposing certain corrections or 
amendments to the text and tables of 40 CFR part 136. EPA is proposing 
adoption of these revisions to improve data quality, update methods to 
keep current with technology advances, and provide the regulated 
community with greater flexibility. The following paragraphs provide 
details on the proposed revisions.

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

    EPA proposes to approve revised versions of the EPA membrane 
filtration methods 1103.2, 1106.2, 1600.1, and 1603.1 found in Tables 
IA and IH. These methods were approved from 2002 to 2014. The revisions 
include standardizing language between the related methods, updating to 
reflect current lab practices and clarifying edits. Copies of these 
proposed method updated versions are available in the docket to this 
rule.
    These methods each describe a membrane filter (MF) procedure for 
the detection and enumeration of either enterococci or Escherichia coli 
bacteria

[[Page 10726]]

by their growth after incubation on selective media. These methods 
provide a direct count of bacteria in water samples based on the 
development of colonies on the surface of the membrane filter.
    1. E. coli. Method 1103.2 describes a MF procedure for the 
detection and enumeration of Escherichia coli bacteria in ambient 
(fresh) water and is currently approved in Table IH. This is a two-step 
method which requires transferring the membrane filter after incubation 
on membrane-Thermotolerant Escherichia coli Agar (mTEC) to a pad 
saturated with urea substrate.
    2. Enterococci. Method 1106.2 describes a MF procedure for the 
detection and enumeration of enterococci bacteria in ambient water and 
is currently approved in Table IH. This is a two-step method which 
requires transferring the membrane filter after incubation on 
membraneEnterococcus (mE) agar to Esculin Iron Agar (EIA) medium.
    3. Enterococci. Method 1600.1 describes a MF procedure for the 
detection and enumeration of enterococci bacteria in ambient (fresh and 
marine) water and wastewater and is currently approved in Tables IA and 
IH. This is a single-step method that is a modification of EPA Method 
1106.1 (mE-EIA). The membrane filter containing the bacterial cells is 
placed on membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI).
    4. E. coli. Method 1603.1 describes a MF procedure for the 
detection and enumeration of thermotolerant Escherichia coli bacteria 
in ambient (fresh) waters and wastewaters using Modified membrane-
Thermotolerant Escherichia coli Agar (modified mTEC) and is currently 
approved in Table IA and IH.

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

    EPA is proposing to approve new versions of ASTM methods previously 
approved in 40 CFR part 136. These changes to currently approved ASTM 
methods in 40 CFR part 136 include minor clarifications and editorial 
changes. As an example, ASTM added text to the appropriate method scope 
sections to indicate that the method was developed in accordance with 
the ``Decision on Principles for the Development of International 
Standards, Guides and Recommendations'' issued by the World Trade 
Organization Technical Barriers to Trade (TBT) Committee. None of these 
proposed changes will affect the performance of the method. The 
following describes the changes to current ASTM methods that EPA 
proposes to include in 40 CFR part 136. Each entry contains (in the 
following order): the parameter, proposed ASTM method number (the last 
two digits in the method number represent the year ASTM published), a 
brief description of the analytical technique, and a brief description 
of any minor procedural changes (if there are any) in this revision 
from the last approved version of the method. Method revisions that are 
only formatting in nature will have no description of the changes. The 
methods listed below are organized according to the table at 40 CFR 
part 136 in the order in which they appear.
    EPA proposes the following changes to ASTM methods found in Table 
IB, and Table II at 40 CFR part 136:
    1. Dissolved Oxygen. D888-18 (A, B, C), Dissolved Oxygen, Winkler, 
Electrode, Luminescent-based Sensor. Standard D888-18A measures 
dissolved oxygen using the Winkler iodometric titration procedure. The 
volume of titrant used is proportional to the concentration of 
dissolved oxygen in the sample. Standard D888-18B measures dissolved 
oxygen in the sample with an electrochemical probe that produces an 
electrical potential which is logarithmically proportional to the 
concentration of dissolved oxygen in the sample. Standard D888-18C 
measures dissolved oxygen with a luminescence-based sensor probe that 
employs frequency domain lifetime-based luminescence quenching and 
signal processing. The 2012 versions, D888-12 (A), (B) and (C), 
currently are approved in Table IB for determination of dissolved 
oxygen.
    2. Hydrogen Ion (pH). In D1293-18 (A, B), pH, Electrometric. The 
activity of hydrogen ion (H+) in the sample is determined 
electrometrically with an ion-selective electrode in comparison to at 
least two standard reference buffers and pH is reported as the negative 
log of that activity. The 1999 version currently is approved in Table 
IB.
    3. Metals Series. In D1976-20, Elements in Water by Inductively-
Coupled Plasma Atomic Emission Spectroscopy for determination of 
aluminum, antimony, arsenic, beryllium, boron, cadmium, chromium, 
cobalt, copper, iron, lead, magnesium, manganese, molybdenum, nickel, 
selenium, silver, thallium, vanadium, and zinc. The sample is acid 
digested and analyzed by inductively-coupled plasma atomic emission 
spectroscopy (ICP/AES) for the simultaneous or sequential determination 
of 29 elements. The changes include changing the initial instrument 
calibration from using four standards as the first option to using only 
one standard and a calibration blank. The 2012 version of this method, 
D1976-12, currently is approved in Table IB for 20 of the 29 elements.
    4. Surfactants. In D2330-20, Methylene Blue Active Substances, the 
sample is mixed with an acidic aqueous solution of methylene blue 
reagent, which forms a blue-colored ion pair with any anionic 
surfactants which is subsequently extracted with chloroform and washed 
with an acidic solution to remove interferences. The intensity of the 
blue color is measured using a photometer at 650 nanometers (nm). The 
concentration of methylene blue active substances is determined in 
comparison to a standard curve. The 2002 version, D2330-02, currently 
is approved in Table IB for determination of surfactants.
    5. Residue, filterable and nonfilterable. In D5907-18 (A and B), 
Filterable Matter (Total Dissolved Solids) and Nonfilterable Matter 
(Total Suspended Solids) under Test Method A, an aliquot of the sample 
is filtered through a glass fiber filter and the solids trapped on the 
filter are dried at 105 [deg]C and weighed to determine the 
nonfilterable material (total suspended solids) by difference. Under 
Test Method B, the filtrate from Test Method A, or a separate filtrate, 
is evaporated to dryness at 180 [deg]C and the residue weighed to 
determine the total dissolved solids. The 2013 version is currently 
approved in Table IB.
    6. Cyanide--Free. In D7237-18, Free Cyanide, Flow Injection, 
followed by Gas Diffusion Amperometry an aliquot of the sample is 
introduced into a flow injection analysis instrument, where it mixes 
with a phosphate buffer to release hydrogen cyanide which diffuses 
through a hydrophobic gas diffusion membrane into an alkaline solution 
and is detected amperometrically with a silver electrode. This version 
also added new information about sulfide interferences and potential 
mitigation strategies that EPA anticipates will improve data quality. 
There are no other procedural changes. The 2015 version, D7237-15, 
currently is approved in Table IB for determination of free cyanide.
    7. Cyanide--Total. In D7284-20, Total Cyanide, Manual Distillation 
with MgCl2 followed by Flow Injection, Gas Diffusion 
Amperometry, the sample is distilled with acid and a magnesium chloride 
catalyst to release cyanide to a sodium hydroxide solution. An aliquot 
of the sodium hydroxide solution is introduced into a flow injection 
analysis instrument, where it is acidified, and

[[Page 10727]]

the hydrogen cyanide diffuses through a hydrophobic gas diffusion 
membrane into an alkaline solution and is detected amperometrically 
with a silver electrode. The 2017 reapproval of D7284-13 currently is 
approved in Table IB for determination of total cyanide.
    8. Organic Carbon. In D7573-18a\e1\, Total Organic Carbon, 
Combustion, the sample is sparged with an inert gas to remove dissolved 
inorganic carbon, acidified, and then combusted at high temperature to 
convert organic carbon to carbon dioxide. The carbon dioxide is 
measured with an infra-red detector. This version also adds data from 
an interlaboratory method validation study and new method detection 
limit values, but there are no procedural changes. The 2017 reapproval 
of D7573-09 currently is approved in Table IB for determination of 
total organic carbon (TOC).

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

    EPA is proposing to approve new versions of methods developed by 
the Standard Methods Committee that were previously approved in 40 CFR 
part 136. Standard Methods has reviewed many of their methods in 
preparation for releasing the next edition of ``Standard Methods for 
the Examination of Water & Wastewater.'' The newer versions provide 
clarifications and make editorial corrections. These edits include 
removal of referents to specific brand names and trademarks, 
incorporation of footnotes into the text, a reformatting of figures, 
tables and reference lists, removal of bibliographical references that 
are no longer available, small editorial changes based on current style 
guides and changes to scientific publishing standards, and minor 
clarifications to procedures based on input from users. For example, 
the revisions replace distilled water with reagent water in all 
methods. As was the case with the previous methods update rule (86 FR 
27226, May 19, 2021), EPA generally proposes to approve and include in 
40 CFR part 136 only the most recent version of a method published by 
the Standard Methods Committee. EPA is proposing to list only one 
version of the method with the year of publication designated by the 
last four digits in the method number (e.g., 3111 C-2019). The date 
indicates the date of the specific revision to the method. This allows 
use of a specific method in any edition of the hard copy publication of 
``Standard Methods for the Examination of Water & Wastewater'' that 
includes a method with the same method number and year of publication.
    The proposed revisions to methods previously approved in 40 CFR 
part 136 will not affect the performance of the method. Below is a list 
of the methods EPA is proposing to include in 40 CFR part 136. Each 
entry contains the proposed Standard Methods number and date, the 
parameter, and a brief description of the analytical method. The 
methods listed below are organized according to the table at 40 CFR 
part 136.
    EPA proposes to make the following changes to Tables IA, IB, IC, ID 
and IH at 40 CFR part 136 for the following parameters:
    1. Color. 2120 B-2021, Visual Comparison Method, is a platinum-
cobalt method of measuring color, the unit of color being that produced 
by one mg platinum per liter in the form of the chloroplatinate ion. 
The 1:2 ratio of cobalt to platinum resulting from the preparation of 
the standard platinum-cobalt solution matches the color of natural 
waters. The 2011 editorial revision currently is approved in Table IB 
for determination of color. 2120 F-2021, American Dye Manufacturers 
Institute (ADMI) Weighted-Ordinate Spectrophotometric Method. In 
accordance with the Adams-Nickerson chromatic value formula, this 
method calculates single-number color difference values (i.e., uniform 
color differences). Values are independent of chroma and hue. 
Transmittance of light is measured spectrophotometrically at multiple 
wavelengths and converted to a set of abstract numbers, which then are 
converted to a single number that indicates color value. This number is 
expressed on a scale used by the ADMI. The 2011 editorial revision 
currently is approved in Table IB for determination of color.
    2. Turbidity. 2130 B-2020, Nephelometric Method is based on a 
comparison of the intensity of light scattered by the sample under 
defined conditions with the intensity of light scattered by a standard 
reference suspension under the same conditions. The higher the 
intensity of scattered light, the higher the turbidity. Formazin 
polymer is used as the primary standard reference suspension. The 2011 
editorial revision currently is approved in Table IB for determination 
of turbidity.
    3. Acidity. 2310 B-2020, Titration Method measures the hydrogen 
ions present in a sample as a result of dissociation or hydrolysis of 
solutes that react with additions of standard alkali. Acidity thus 
depends on the endpoint pH or indicator used. The construction of a 
titration curve by recording a sample's pH after successive small, 
measured additions of titrant permits identification of inflection 
points and buffering capacity, if any, and allows the acidity to be 
determined with respect to any pH of interest. Samples of industrial 
wastes, acid mine drainage, or other solutions that contain appreciable 
amounts of hydrolyzable metal ions such as iron, aluminum, or manganese 
are treated with hydrogen peroxide to ensure the oxidation of any 
reduced forms of polyvalent cations and are boiled to hasten 
hydrolysis. Acidity results may be highly variable if this procedure is 
not followed exactly. The 2011 editorial revision currently is approved 
in Table IB for determination of acidity.
    4. Alkalinity. 2320 B-2021 Titration Method, measures the hydroxyl 
ions present in a sample resulting from dissociation or hydrolysis of 
solutes that react with additions of standard acid. Alkalinity thus 
depends on the endpoint pH used. For samples of low alkalinity (less 
than 20 mg/L CaCO3) an extrapolation technique based on the 
near proportionality of concentration of hydrogen ions to excess of 
titrant beyond the equivalence point is used. The amount of standard 
acid required to reduce the pH exactly 0.30 pH unit is measured 
carefully. Because this change in pH corresponds to an exact doubling 
of the hydrogen ion concentration, a simple extrapolation can be made 
to the equivalence point. The 2011 editorial revision currently is 
approved in Table IB for determination of alkalinity.
    5. Hardness. 2340 B-2021, Hardness by Calculation is the preferred 
method for determining hardness by calculating it from the results of 
separate determinations of calcium and magnesium by any approved method 
provided that the sum of the lowest point of quantitation for Ca and Mg 
is below the NPDES permit requirement for hardness. The 2011 editorial 
revision currently is approved in Table IB for determination of 
hardness. In 2340 C-2021, Ethylenediaminetetraacetic acid (EDTA) 
Titrimetric Method, EDTA forms a chelated soluble complex when added to 
a solution of certain metal cations. If a small amount of a dye such as 
eriochrome black T or calmagite is added to an aqueous solution 
containing calcium and magnesium ions at a pH of 10.0  0.1, 
the color of the solution becomes wine red. If EDTA is added as a 
titrant, the calcium and magnesium will be complexed, and when all of 
the magnesium and calcium has been complexed, the solution turns from 
wine red to blue, marking the endpoint of the titration. The volume of 
titrant used is proportional to hardness in the

[[Page 10728]]

sample. Magnesium ion must be present to yield a satisfactory endpoint. 
To ensure this, a small amount of complexometrically neutral magnesium 
salt of EDTA is added to the buffer; this automatically introduces 
sufficient magnesium and obviates the need for a blank correction. The 
2011 editorial revision currently is approved in Table IB for 
determination of hardness.
    6. Specific Conductance. 2510 B-2021 measures conductance (or 
resistance) in the laboratory using a standard potassium chloride 
solution and from the corresponding conductivity, a cell constant is 
calculated. Most conductivity meters do not display the actual solution 
conductance, or resistance, rather, they generally have a dial that 
permits the user to adjust the internal cell constant to match the 
conductivity of a standard. Once the cell constant has been determined, 
or set, the conductivity of an unknown solution is displayed by the 
meter. The 2011 editorial revision currently is approved in Table IB 
for determination of specific conductance.
    7. Residue--Total. In 2540 B-2020 an aliquot of a well-mixed sample 
is evaporated in a pre-weighed evaporating dish at 103-105 [deg]C to 
constant weight in a 103 to 105 [deg]C oven. The increase compared to 
the empty pre-weighed dish weight represents total solids. The 2015 
version of the method currently is approved in Table IB for 
determination of total residue. In 2540 C-2020, Total Dissolved Solids 
Dried at 180 [deg]C (Residue--filterable in Table IB) a measured volume 
of a well-mixed sample is filtered through a glass fiber filter with 
applied vacuum. The entire exposed surface of the filter is washed with 
at least 3 successive volumes of reagent-grade water with continued 
suction until all traces of water are removed. The total filtrate (with 
washings) is then transferred to a pre-weighed dish and evaporated to 
dryness. Successive volumes of sample are added to the same dish after 
evaporation if necessary to yield between 2.5 and 200 mg of dried 
residue. The evaporated residue is then dried for one hour or more in 
an oven at 180 [deg]C, cooled in a desiccator to ambient temperature, 
and weighed until the weight change is less than 0.5 mg. The 2015 
version of the method currently is approved in Table IB for 
determination of filterable residue. In 2540 D-2020, Total Suspended 
Solids Dried from 103 to 105 [deg]C (Residue--non-filterable total 
suspended solids (TSS) in Table IB) a well-mixed sample is filtered 
through a pre-weighed standard glass-fiber filter. The filter and the 
retained residue are then dried to a constant weight in a 103 to 105 
[deg]C oven. The increase in filter weight represents TSS. The 2015 
version of the method currently is approved in Table IB for 
determination of non-filterable residue. In 2540 E-2020, Fixed and 
Volatile Solids Ignited at 550 [deg]C (Residue--volatile in Table IB) 
the residue obtained from the determination of total (Method 2540 B), 
filterable (Method 2540 C), or non-filterable residue (Method 2540 D) 
is ignited at 550  50 [deg]C in a muffle furnace, cooled in 
a desiccator to ambient temperature and weighed. Repeated successive 
cycles of drying, cooling, desiccating, and weighing are performed 
until the weight change is less than 0.5 mg. The remaining solids are 
fixed total, dissolved, or suspended solids, while those lost to 
ignition are volatile total, dissolved, or suspended solids. The 2015 
version of the method currently is approved in Table IB for 
determination of volatile residue. In 2540 F-2020, Settleable Solids 
(aka, Residue--settleable in Table IB), a well-mixed sample is used to 
fill an Imhoff cone or graduated cylinder to the 1-L mark. The sample 
is allowed to settle for 45 minutes, then gently agitated near the 
sides of the cone (or graduated cylinder) with a rod or by spinning. 
The sample is then allowed to settle for another 15 minutes and the 
volume of settleable solids in the cone (or graduated cylinder) is 
recorded as mL/L. When applicable, the recorded volume is corrected for 
interference from pockets of liquid volume. The 2015 version of the 
method currently is approved in Table IB for determination of 
settleable residue.
    8. Multiple metals by flame atomic absorption spectrometry.
    a. 3111 B-2019, Direct Air-Acetylene Flame Method. The 2011 
editorial revision currently is approved in Table IB for determination 
of antimony, cadmium, calcium, chromium, cobalt, copper, gold, iridium, 
iron, lead, magnesium, manganese, nickel, palladium, platinum, 
potassium, rhodium, ruthenium, silver, sodium, thallium, tin, and zinc. 
A sample is aspirated into a flame and the metals are atomized. A light 
beam is directed through the flame, into a monochromator, and onto a 
detector that measures the amount of light absorbed by the atomized 
metal in the flame. Because each metal has its own characteristic 
absorption wavelength, a source lamp composed of that element is used. 
The amount of energy at the characteristic wavelength absorbed in the 
flame is proportional to the concentration of the element in the sample 
over a limited concentration range.
    b. 3111 C-2019, Extraction and Air-Acetylene Flame Method consists 
of chelation with ammonium pyrrolidine dithiocarbamate (APDC) and 
extraction into methyl isobutyl ketone (MIBK), followed by aspiration 
into an air-acetylene flame and is suitable for the determination of 
low concentrations of cadmium, chromium, cobalt, copper, iron, lead, 
manganese, nickel, silver, and zinc. The 2011 editorial revision 
currently is approved in Table IB for determination of cadmium, 
chromium, cobalt, copper, iron, lead, nickel, silver, and zinc.
    EPA proposes to approve method 3111 C for manganese. This parameter 
was inadvertently left off in an earlier rulemaking approving method 
3111 C.
    c. 3111 D-2019, Direct Nitrous Oxide-Acetylene Flame Method. A 
sample is aspirated into a flame produced using a mixture of nitrous 
oxide and acetylene and the metals are atomized. A light beam is 
directed through the flame, into a monochromator, and onto a detector 
that measures the amount of light absorbed by the atomized metal in the 
flame. The 2011 editorial revision currently is approved in Table IB 
for determination of aluminum, barium, beryllium, molybdenum, osmium, 
titanium, and vanadium. In addition, EPA proposes to approve method 
3111 D for calcium. This parameter was inadvertently left off in an 
earlier rulemaking approving method 3111 D.
    d. 3111 E-2019, Extraction and Nitrous Oxide-Acetylene Flame 
Method. The method consists of chelation with 8-hydroxyquinoline, 
extraction with MIBK, and aspiration into a nitrous oxide-acetylene 
flame and is suitable for the determination of aluminum at 
concentrations less than 900 [mu]g/L and beryllium at concentrations 
less than 30 [mu]g/L. The 2011 editorial revision currently is approved 
in Table IB for determination of aluminum, and beryllium.
    9. Mercury--Total. 3112 B-2020, Metals by Cold-Vapor Atomic 
Absorption Spectrometric Method is a flameless AA procedure based on 
the absorption of radiation at 253.7 nm by mercury vapor. The mercury 
in a sample is reduced to the elemental state and aerated from solution 
in a closed system. The mercury vapor passes through a cell positioned 
in the light path of an atomic absorption spectrophotometer. Absorbance 
is measured as a function of mercury concentration. The 2011 editorial 
revision currently is approved in Table IB for determination of 
mercury.

[[Page 10729]]

    10. Metals by AA Furnace. In 3113 B-2020, Electrothermal Atomic 
Absorption Spectrometric Method, a discrete sample volume is dispensed 
into the graphite sample tube (or cup). Typically, determinations are 
made by heating the sample in three or more stages. First, a low 
current heats the tube to dry the sample. The second, or charring, 
stage destroys organic matter and volatilizes other matrix components 
at an intermediate temperature. Finally, a high current heats the tube 
to incandescence and, in an inert atmosphere, atomizes the element 
being determined. Additional stages frequently are added to aid in 
drying and charring, and to clean and cool the tube between samples. 
The resultant ground-state atomic vapor absorbs monochromatic radiation 
from the source. A photoelectric detector measures the intensity of 
transmitted radiation. The inverse of the transmittance is related 
logarithmically to the absorbance, which is directly proportional to 
the number density of vaporized ground-state atoms (the Beer-Lambert 
law) over a limited concentration range. The 2010 version of the method 
currently is approved in Table IB for determination of aluminum, 
antimony, arsenic, barium, beryllium, cadmium, chromium, cobalt, 
copper, iron, lead, manganese, molybdenum, nickel, selenium, silver, 
and tin. Although not specifically listed as target analytes in 3113 B, 
the 2010 version of the method is also approved in Table IB for 
determination of gold, thallium, and vanadium, as these elements may 
also be determined using the method.
    11. Arsenic and Selenium by AA Gaseous Hydride. 3114 B-2020, Manual 
Hydride Generation/Atomic Absorption Spectrometric Method is a manual 
hydride generation method that is applicable to the determination of 
arsenic and selenium by conversion to their hydrides by sodium 
borohydride reagent and transport into an atomic absorption atomizer. 
The 2011 editorial revision currently is approved in Table IB for 
determination of arsenic and selenium. 3114 C-2020, Continuous Hydride 
Generation/Atomic Absorption Spectrometric Method is a continuous-flow 
hydride generation method that is applicable to the determination of 
arsenic and selenium by conversion to their hydrides by sodium 
borohydride reagent and transport into an atomic absorption atomizer. 
The continuous hydride generator offers the advantages of simplicity in 
operation, excellent reproducibility, low detection limits, and high 
sample volume throughput for selenium analysis following preparations 
as described in 3500-Se B or 3114 B.4c and d. The 2011 editorial 
revision currently is approved in Table IB for determination of arsenic 
and selenium.
    12. Multiple Metals by ICP/AES (Plasma Emission Spectroscopy). In 
3120 B-2020, an Inductively Coupled Plasma (ICP) source consists of a 
flowing stream of argon gas ionized by an applied radio frequency field 
typically oscillating at 27.1 MHz. This field is inductively coupled to 
the ionized gas by a water-cooled coil surrounding a quartz torch that 
supports and confines the plasma. A sample aerosol is generated in an 
appropriate nebulizer and spray chamber and is carried into the plasma 
through an injector tube located within the torch. The sample aerosol 
is injected directly into the ICP, subjecting the constituent atoms to 
temperatures of about 6000 to 8000 [deg]K. Because this results in 
almost complete dissociation of molecules, significant reduction in 
chemical interferences is achieved. The high temperature of the plasma 
excites atomic emission efficiently. Ionization of a high percentage of 
atoms produces ionic emission spectra. The ICP provides an optically 
thin source that is not subject to self-absorption except at very high 
concentrations. Total metals are determined after appropriate 
digestion. The 2011 editorial revision currently is approved in Table 
IB for determination of aluminum, antimony, arsenic, barium, beryllium, 
boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, 
magnesium, manganese, molybdenum, nickel, potassium, selenium, silica, 
silver, sodium, thallium, vanadium, and zinc. Although not specifically 
listed as a target analyte in method 3120 B, the 2011 version of the 
method is also approved in Table IB for determination of phosphorus 
because this element may also be determined using the method.
    13. Multiple Metals by Inductively Coupled Plasma-Mass 
Spectrometry. In this method, 3125 B-2020, Inductively Coupled Plasma-
Mass Spectrometry (ICP-MS) Method, a sample is introduced into an 
argon-based, high-temperature radio-frequency plasma, usually via 
pneumatic nebulization. As energy transfers from the plasma to the 
sample stream, the target element desolvation, atomization, and 
ionization. The resulting ions are extracted from the plasma through a 
differential vacuum interface and separated based on their mass-to-
charge (m/z) ratio by a mass spectrometer. Typically, either a 
quadrupole (with or without collision cell technology or dynamic 
reaction cell) or magnetic sector (high-resolution) mass spectrometer 
is used. An electron multiplier detector counts the separated ions, and 
a computer-based data-management system processes the resulting 
information. The 2011 editorial revision currently is approved in Table 
IB for determination of aluminum, antimony, arsenic, barium, beryllium, 
cadmium, chromium, cobalt, copper, lead, manganese, molybdenum, nickel, 
potassium, selenium, silver, thallium, vanadium, and zinc. Although not 
specifically listed as a target analyte in method 3125 B, the 2011 
version of the method is also approved in Table IB for determination of 
boron, calcium, gold, iridium, iron, magnesium, palladium, platinum, 
potassium, rhodium, ruthenium, silica, sodium, tin, and titanium as 
these elements may also be determined using the method.
    14. 3500 Colorimetric Series for Multiple Metals.
    a. Aluminum. In 3500-Al B-2020, Eriochrome Cyanine R Method with 
Eriochrome cyanine R dye, dilute aluminum solutions buffered to a pH of 
6.0 produce a red to pink complex that exhibits maximum absorption at 
535 nm. The intensity of the developed color is influenced by the 
aluminum concentration, reaction time, temperature, pH, alkalinity, and 
concentration of other ions in the sample. To compensate for color and 
turbidity, the aluminum in one portion of a sample is complexed with 
EDTA to provide a blank. The interference of iron and manganese, two 
elements commonly found in water when aluminum is present, is 
eliminated by adding ascorbic acid. The 2011 editorial revision 
currently is approved in Table IB for determination of aluminum.
    b. Arsenic. In 3500-As B-2020, Silver Diethyldithiocarbamate 
Method, arsenite, containing trivalent arsenic, is reduced selectively 
by aqueous sodium borohydride solution to arsine, AsH3, in 
an aqueous medium of pH 6. Arsenate, methylarsonic acid, and 
dimethylarsinic acid are not reduced under these conditions. The 
generated arsine is swept by a stream of oxygen-free nitrogen from the 
reduction vessel through a scrubber containing glass wool or cotton 
impregnated with lead acetate solution into an absorber tube containing 
silver diethyldithiocarbamate and morpholine dissolved in chloroform. 
The intensity of the red color that develops is measured at 520 nm. The 
2011 editorial revision currently is approved in Table IB for 
determination of arsenic.
    c. Calcium. In 3500-Ca B-2020, EDTA Titrimetric Method, EDTA is 
added to water containing both calcium and

[[Page 10730]]

magnesium, where it combines first with the calcium. Calcium can be 
determined directly, with EDTA, when the pH is made sufficiently high 
that the magnesium is largely precipitated as the hydroxide and an 
indicator is used that combines with calcium only. Several indicators 
give a color change when all the calcium has been complexed by the EDTA 
at a pH of 12 to 13. The 2011 editorial revision currently is approved 
in Table IB for determination calcium.
    d. Chromium. 3500-Cr B-2020, Colorimetric Method. This procedure 
measures only hexavalent chromium, (chromium VI). The hexavalent 
chromium is determined colorimetrically by reaction with 
diphenylcarbazide in acid solution. A red-violet colored complex of 
unknown composition is produced. The 2011 editorial revision currently 
is approved in Table IB for determination of dissolved hexavalent 
chromium (chromium VI). 3500-Cr C-2020, Ion Chromatographic Method. 
This method is applicable to determination of dissolved hexavalent 
chromium in drinking water, groundwater, and industrial wastewater 
effluents. An aqueous sample is filtered, and its pH adjusted to 
between 9 and 9.5 with a concentrated buffer. This pH adjustment 
reduces the solubility of trivalent chromium and preserves the 
hexavalent chromium oxidation state. The sample is introduced into the 
instrument's eluent stream of ammonium sulfate and ammonium hydroxide. 
Trivalent chromium in solution is separated from the hexavalent 
chromium by the column. After separation, hexavalent chromium reacts 
with an azide dye to produce a chromogen that is measured at 530 or 540 
nm. Hexavalent chromium is identified based on retention time. The 2011 
editorial revision currently is approved in Table IB for determination 
of dissolved hexavalent chromium (chromium VI).
    e. Copper Colorimetric. In 3500-Cu B-2020, Neocuproine Method, the 
sample is treated with hydroxylamine hydrochloride to reduce any cupric 
ions (Cu\2+\) to cuprous ions (Cu\+\). Sodium citrate is used to 
complex metallic ions that might precipitate when the pH is raised. The 
pH is adjusted to between 4 and 6 with ammonium hydroxide 
(NH4OH), a solution of neocuproine (2,9-dimethyl-1,10-
phenanthroline) in methanol is added, and the resultant complex is 
extracted into chloroform (CHCl3). After dilution of the 
CHCl3 to an exact volume with methanol (CH3OH), 
the absorbance of the solution is measured at 457 nm. The 2011 
editorial revision currently is approved in Table IB for determination 
of copper. In 3500-Cu C-2020, Bathocuproine Method, cuprous ion forms a 
water-soluble orange-colored chelate with disodium bathocuproine 
disulfonate (sodium 4,4'-(2,9-dimethyl-1,10-phenanthroline-4,7-
diyl)dibenzenesulfonate). While the color forms over the pH range 3.5 
to 11.0, the recommended pH range is between 4 and 5. The sample is 
buffered at a pH of about 4.3 and reduced with hydroxylamine 
hydrochloride. The absorbance is measured at 484 nm. The 2011 editorial 
revision currently is approved in Table IB for determination of copper.
    f. Potassium. In 3500-K B-2020, Flame Photometric Method, trace 
amounts of potassium can be determined in either a direct-reading or 
internal-standard type of flame photometer at a wavelength of 766.5 nm. 
The 2011 editorial revision currently is approved in Table IB for 
determination of potassium. In 3500-K C-2020, Potassium-Selective 
Electrode Method, potassium ions are measured potentiometrically by 
using a potassium ion-selective electrode and a double-junction, 
sleeve-type reference electrode. The analysis is performed with either 
a pH meter having an expanded millivolt scale capable of being read to 
the nearest 0.1 mV or a specific-ion meter having a direct 
concentration scale for potassium. Before measurement, an ionic 
strength adjustor reagent is added to both standards and samples to 
maintain a constant ionic strength. The electrode response is measured 
in standard solutions with potassium concentrations spanning the range 
of interest using a calibration line derived either by the instrument 
meter or manually. The electrode response in sample solutions is 
measured following the same procedure and potassium concentration 
determined from the calibration line or instrument direct readout. The 
2011 editorial revision currently is approved in Table IB for 
determination of potassium.
    g. Manganese. In 3500-Mn B-2020, Persulfate Method, persulfate 
oxidation of soluble manganous compounds to form permanganate is 
carried out in the presence of silver nitrate. The resulting color is 
stable for at least 24 hours if excess persulfate is present and 
organic matter is absent. The 2011 editorial revision currently is 
approved in Table IB for determination of manganese.
    h. Sodium. In 3500-Na B-2020, Flame Emission Photometric Method a 
sample is nebulized into a gas flame under carefully controlled, 
reproducible excitation conditions. The sodium resonant spectral line 
at 589 nm is isolated by interference filters or by light-dispersing 
devices such as prisms or gratings. Emission light intensity is 
measured by a phototube, photomultiplier, or photodiode. The light 
intensity at 589 nm is approximately proportional to the sodium 
concentration. The 2011 editorial revision currently is approved in 
Table IB for determination of sodium.
    i. Lead. In 3500-Pb B-2020, Dithizone Method, an acidified sample 
containing microgram quantities of lead is mixed with ammoniacal 
citrate-cyanide reducing solution and extracted with dithizone in 
chloroform (CHCl3) to form a cherry-red lead dithizonate. 
The color of the mixed color solution is measured photometrically. The 
2011 editorial revision currently is approved in Table IB for 
determination of lead.
    j. Zinc. 3500-Zn B-2020, Zincon Method. Zinc forms a blue complex 
with zincon (2-carboxy-2'-hydroxy-5'-sulfoformazyl benzene) in a 
solution buffered to pH 9.0. Other heavy metals likewise form colored 
complexes with zincon. Cyanide is added to complex zinc and heavy 
metals. Cyclohexanone is added to selectively free zinc from its 
cyanide complex so that it can be complexed with zincon to form a blue 
color which is measured spectrophotometrically at 620 nm. Sodium 
ascorbate reduces manganese interference. The developed color is stable 
except in the presence of copper. The 2011 editorial revision currently 
is approved in Table IB for determination of zinc.
    15. 4110 Series, Ion Chromatography.
    a. In 4110 B-2020, Ion Chromatography with Chemical Suppression of 
Eluent Conductivity, is approved in Table IB for determination of 
bromide, chloride, fluoride, nitrate, nitrite, orthophosphate, and 
sulfate. A water sample is injected into a stream of eluent and passed 
through a series of ion exchangers. The anions of interest are 
separated based on their relative affinities for a low-capacity, 
strongly basic anion exchanger (guard and analytical columns). The 
separated anions are directed through a suppressor device that provides 
continuous suppression of eluent conductivity and enhances analyte 
response. In the suppressor, the separated anions are converted to 
their highly conductive acid forms while the conductivity of the eluent 
is greatly decreased. The separated anions in their acid forms are 
measured by conductivity. They are identified based on retention time 
as compared to standards. Quantitation is by measurement of peak area 
or peak height. The 2011 editorial revision

[[Page 10731]]

currently is approved in Table IB for determination of bromide, 
chloride, fluoride, nitrate, combined nitrate-nitrite, nitrite, 
orthophosphate, and sulfate.
    b. 4110 C-2020, Single-Column Ion Chromatography with Direct 
Conductivity Detection. An aqueous sample is injected into an ion 
chromatograph consisting of an injector port, analytical column, and 
conductivity detector. The sample merges with the eluent stream and is 
pumped through the analytical column where the anions are separated 
based on their affinity for the active sites of the column packing 
material. Concentrations are determined by direct conductivity 
detection without chemical suppression. The 2011 editorial revision 
currently is approved in Table IB for determination of bromide, 
chloride, fluoride, nitrate, combined nitrate-nitrite, nitrite, 
orthophosphate, and sulfate.
    c. 4110 D-2020, Ion Chromatographic Determination of Oxyhalides and 
Bromide. The sample is analyzed in a manner similar to that in 4110 B-
2020. However, bromate has been shown to be subject to positive 
interferences in some matrices. The interference is noticeable usually 
as a flattened peak. It often can be eliminated by passing the sample 
through an H\+\ off-line solid-phase extraction (SPE) cartridge, by 
selection of a different column-eluent combination, or by diluting the 
eluent, which will increase retention times and spread the 
chromatogram. Additionally, chloride or a nontarget analyte present in 
unusually high concentration may overlap with a target analyte 
sufficiently to cause problems in quantitation or may cause retention-
time shifts. Dilution of the sample may resolve this problem. The 2011 
editorial revision currently is approved in Table IB for determination 
of bromide.
    16. Inorganic Anions by CIE/UV (Capillary Ion Electrophoresis). In 
4140 B-2020, Capillary Ion Electrophoresis with Indirect UV Detection, 
the sample is introduced at the cathodic end of the capillary and 
anions are separated based on their differences in mobility in the 
electric field as they migrate through the capillary. Cations migrate 
in the opposite direction and are not detected. Water and neutral 
organics are not attracted toward the anode. They migrate after the 
anions and thus do not interfere with anion analysis. Anions are 
detected as they displace charge-for-charge the UV-absorbing 
electrolyte anion (chromate), causing a net decrease in UV absorbance 
in the analyte anion zone compared to the background electrolyte. 
Detector polarity is reversed to provide positive millivolt response to 
the data system. As in chromatography, the analytes are identified by 
their migration time and quantitated by using time-corrected peak area 
relative to standards. The 2011 editorial revision currently is 
approved in Table IB for determination of bromide, chloride, fluoride, 
nitrate, combined nitrate-nitrite, nitrite, orthophosphate, and 
sulfate.
    17. 4500 Series, Chloride.
    a. 4500-Cl- B-2021, Titrimetric Method. In a neutral or 
slightly alkaline solution, potassium chromate can indicate the 
endpoint of the silver nitrate titration of chloride. Silver chloride 
is precipitated quantitatively before red silver chromate is formed. In 
this version of the method approved by the Standard Methods Committee 
in 2021, additional information regarding removal of interferences 
caused by sulfide, thiosulfate, and sulfite ions by digestion of the 
sample with hydrogen peroxide prior to titration has been added to the 
sample preparation procedures. A tighter pH range of 8-10, as opposed 
to 7-10, is specified for adjustment of the pH of the sample prior to 
titration. A reference has been added for the 2021 Standard Methods 
Joint Task Group validation report titled: ``Interlaboratory validation 
study for the use of H2O2 with boiling for 
determining Cl-.'' The 2011 editorial revision currently is 
approved in Table IB for determination of chloride.
    b. 4500-Cl- C-2021, Mercuric Nitrate Method. Chloride 
can be titrated with mercuric nitrate, Hg(NO3)2, 
because of the formation of soluble, slightly dissociated mercuric 
chloride. In the pH range 2.3 to 2.8, diphenylcarbazone indicates the 
titration endpoint by formation of a purple complex with the excess 
mercuric ions. Xylene cyanol FF serves as a pH indicator and endpoint 
enhancer. Increasing the strength of the titrant and modifying the 
indicator mixtures extend the range of measurable chloride 
concentrations. The 2011 editorial revision currently is approved in 
Table IB for determination of chloride.
    c. 4500-Cl- D-2021, Potentiometric Method. Chloride is 
determined by potentiometric titration with silver nitrate solution 
with a glass and silver-silver chloride electrode system. During 
titration, an electronic voltmeter is used to detect the change in 
potential between the two electrodes. The endpoint of the titration is 
that instrument reading at which the greatest change in voltage has 
occurred for a small and constant increment of silver nitrate added. 
The 2011 editorial revision currently is approved in Table IB for 
determination of chloride.
    d. 4500-Cl- E-2021, Automated Ferricyanide Method. 
Thiocyanate ion is liberated from mercuric thiocyanate by the formation 
of soluble mercuric chloride. In the presence of ferric ion, free 
thiocyanate ion forms a highly colored ferric thiocyanate, of which the 
intensity is proportional to the chloride concentration. The 2011 
editorial revision currently is approved in Table IB for determination 
of chloride.
    18. 4500 Series Cyanide Total or Available.
    a. 4500-CN- B-2021, Manual Distillation (as Preliminary 
Treatment of Samples). Total cyanides are measured after preliminary 
treatment of samples for preservation and to remove interferences. The 
preliminary treatment required depends on which interfering substances 
the samples contain. Distillation removes many interfering substances, 
but other pretreatment procedures will be needed for sample containing 
sulfides, fatty acids, oxidizing agents, nitrites, and nitrates. The 
2016 version of the method currently is approved in Table IB for 
preliminary treatment of samples to be used for determination of 
cyanide.
    b. 4500-CN- C-2021, Total Cyanide after Distillation. 
Hydrogen cyanide (HCN) is liberated from an acidified sample by 
distillation and purging with air, with the HCN gas collected in a NaOH 
scrubbing solution. The cyanide concentration in the scrubbing solution 
is determined via titrimetric, colorimetric, or potentiometric 
procedures. The 2016 version of the method currently is approved in 
Table IB for preliminary treatment of samples to be used for 
determination of cyanide.
    c. 4500-CN- D-2021, Titrimetric Method. CN- 
in the alkaline distillate from the preliminary treatment procedures 
(4500-CN- B and C) is titrated with standard silver nitrate 
(AgNO3) to form the soluble cyanide complex 
Ag(CN)2-. As soon as all CN- has been 
complexed and a small excess of Ag\+\ has been added, the silver-
sensitive indicator, p-dimethylaminobenzalrhodanine, detects the excess 
Ag\+\ and immediately changes color from yellow to salmon. The 2016 
version of the method currently is approved in Table IB for 
determination of cyanide.
    d. 4500-CN- E-2021, Spectrophotometric Method. Total 
CN- in the alkaline distillate from the preliminary 
treatment procedures (4500-CN- B and C) is converted to 
cyanogen chloride (CNCl) by reaction with chloramine-T at pH <8 without 
hydrolyzing to cyanate (CNO-). After

[[Page 10732]]

the reaction is complete, adding a pyridine-barbituric acid reagent 
turns CNCl a red-blue color. Maximum color absorbance in aqueous 
solution is between 575 and 582 nm. The 2016 version of the method 
currently is approved in Table IB for determination of cyanide.
    e. 4500-CN- F-2021, Ion Selective Electrode Method. 
Total CN- in the alkaline distillate from the preliminary 
treatment procedures (4500-CN- B and C) is determined 
potentiometrically by using a CN--ion selective electrode. 
The 2016 version of the method currently is approved in Table IB for 
determination of cyanide.
    f. 4500-CN- G-2021, Cyanides Amenable to Chlorination 
after Distillation. Available cyanide, or cyanide amenable to 
chlorination (CATC), can be determined when a portion of the sample is 
chlorinated at high pH and cyanide levels in the chlorinated sample are 
determined after manual distillation followed by titrimetric or 
spectrophotometric measurement. CATC is calculated by the difference 
between the results for cyanide in the unchlorinated sample and the 
results for the chlorinated sample. The 2016 version of the method 
currently is approved in Table IB for preliminary treatment of samples 
to be used for determination of available cyanide.
    g. 4500-CN- N-2021, Total Cyanide after Distillation by 
Flow Injection Analysis. Total cyanides are digested and steam-
distilled from the sample (4500-CN- C), The cyanide in this 
distillate is converted to CNCl by reaction with chloramine-T at pH <8. 
The CNCl then forms a red-blue dye by reacting with pyridine-barbituric 
acid reagent. The absorbance of this red dye is measured at 570 nm and 
is proportional to the total or weak acid dissociable cyanide in the 
sample. The 2016 version of the method currently is approved in Table 
IB for determination of cyanide.
    19. 4500 Total Fluoride Series.
    a. 4500-F- B-2021, Preliminary Distillation Step. 
Fluoride is separated from other nonvolatile constituents in water by 
conversion to hydrofluoric or fluosilicic acid and subsequent 
distillation. The conversion is accomplished by using a strong, high-
boiling acid. To protect against glassware etching, hydrofluoric acid 
is converted to fluosilicic acid by using soft glass beads. 
Quantitative fluoride recovery is accomplished by using a relatively 
large sample. Acid and sulfate carryover are minimized by distilling 
over a controlled temperature range. The 2011 editorial revision 
currently is approved in Table IB for preliminary treatment of samples 
to be used for determination of fluoride.
    b. 4500-F- C-2021, Ion-Selective Electrode Method. The 
fluoride electrode is an ion-selective sensor that measures the ion 
activity of fluoride in solution rather than concentration. The key 
element in the fluoride electrode is the laser-type doped lanthanum 
fluoride crystal across which a potential is established by fluoride 
solutions of different concentrations. The crystal contacts the sample 
solution at one face and an internal reference solution at the other. 
Fluoride ion activity depends on the solution total ionic strength and 
pH, and on fluoride complexing species. Adding an appropriate buffer 
provides a nearly uniform ionic strength background, adjusts pH, and 
breaks up complexes. In effect, the electrode measures concentration. 
The 2011 editorial revision currently is approved in Table IB for 
determination of fluoride.
    c. 4500-F- D-2021, SPADNS Method. The SPADNS 
colorimetric method is based on the reaction between fluoride and a 
``lake'' of zirconium-dye. Fluoride reacts with the dye lake, 
dissociating a portion of it into a colorless complex anion 
(ZrF62-) and the dye. As the amount of fluoride 
increases, the color produced becomes progressively lighter and 
absorbance is measured colorimetrically at 570 nm. The 2011 editorial 
revision currently is approved in Table IB for determination of 
fluoride.
    d. 4500-F- E-2021, Complexone Method. The sample is 
distilled in the automated system, and the distillate is reacted with 
alizarin fluorine blue-lanthanum reagent to form a blue complex that is 
measured colorimetrically at 620 nm. The 2011 editorial revision 
currently is approved in Table IB for determination of fluoride.
    20. 4500 Hydrogen ion (pH). 4500-H\+\ B-2021, Electrometric Method. 
The basic principle of electrometric pH measurement is determination of 
the activity of the hydrogen ions by potentiometric measurement using a 
standard hydrogen electrode and a reference electrode. The hydrogen 
electrode consists of a platinum electrode across which hydrogen gas is 
bubbled at a pressure of 101 kilopascal. Because of difficulty in its 
use and the potential for poisoning the hydrogen electrode, the glass 
electrode commonly is used. The electromotive force (emf) produced in 
the glass electrode system varies linearly with pH. This linear 
relationship is described by plotting the measured emf against the pH 
of different buffers. A sample's pH is determined by extrapolation. 
This version of the method adds information to Section 2--Apparatus, 
regarding equipment that may be used for manual or automatic 
temperature compensation. The 2011 editorial revision currently is 
approved in Table IB for determination of pH.
    21. 4500 Kjeldahl Nitrogen (TKN) Series.
    a. 4500-Norg B-2021, Macro-Kjeldahl Method. In the presence of 
sulfuric acid (H2SO4), potassium sulfate 
(K2SO4), and a cupric sulfate (CuSO4) 
catalyst, amino nitrogen of many organic materials is converted to 
ammonium. Free ammonia also is converted to ammonium. After the 
addition of base, the ammonia is distilled from an alkaline medium and 
absorbed in boric or sulfuric acid. The ammonia may be determined 
colorimetrically, by ammonia-selective electrode, or by titration with 
a standard mineral acid. The 2011 editorial revision currently is 
approved in Table IB for preliminary treatment of samples to be used 
for determination of total Kjeldahl nitrogen (TKN).
    b. 4500-Norg C-2021, Semi-Micro-Kjeldahl Method. This is a reduced-
volume version of 4500 Norg B that specifies use of Kjeldahl 
flasks with a capacity of 100 mL in a semi-micro-Kjeldahl digestion 
apparatus equipped with heating elements to accommodate Kjeldahl flasks 
and a suction outlet to vent fumes. The 2011 editorial revision 
currently is approved in Table IB for preliminary treatment of samples 
to be used for determination of total Kjeldahl nitrogen (TKN).
    c. 4500-Norg D-2021, Block Digestion and Flow Injection Analysis. 
Samples are digested in a block digestor with sulfuric acid and copper 
sulfate as a catalyst. The digested sample is injected onto the FIA 
manifold, where its pH is controlled by raising it to a known, basic pH 
by neutralization with a concentrated buffer. This in-line 
neutralization converts the ammonium cation to ammonia, and also 
prevents undue influence of the sulfuric acid matrix on the pH-
sensitive color reaction that follows. The ammonia thus produced is 
heated with salicylate and hypochlorite to produce a blue color that is 
proportional to the ammonia concentration. The color is intensified by 
adding sodium nitroprusside. The presence of EDTA in the buffer 
prevents the precipitation of calcium and magnesium. The resulting 
peak's absorbance is measured at 660 nm. The peak area is proportional 
to the concentration of total Kjeldahl nitrogen in the original sample. 
The 2011 editorial revision currently is approved

[[Page 10733]]

in Table IB for determination of total Kjeldahl nitrogen.
    22. 4500-NH3 Nitrogen (Ammonia as nitrogen) Series.
    a. 4500-NH3 B-2021, Preliminary Manual Distillation Step. The 
sample is buffered at pH 9.5 with a borate buffer to decrease 
hydrolysis of cyanates and organic nitrogen compounds. It is distilled 
into a solution of boric acid when titration is to be used, or into 
H2SO4, when the phenate method is used as the 
determinative step. The ammonia in the distillate can be determined 
either colorimetrically by the phenate method or titrimetrically with 
standard H2SO4 and a mixed indicator or a pH 
meter. Ammonia in the distillate also can be determined by the ammonia-
selective electrode method, using 0.04 N H2SO4 to 
trap the ammonia. This revision replaces instructions for storage of 
ammonia-free water with instructions for preparation of ammonia-free 
water using an ion exchange resin and simply says that if high blank 
values are produced, the analyst should prepare fresh ammonia-free 
water. The 2011 editorial revision currently is approved in Table IB 
for preliminary treatment of samples to be used for determination of 
ammonia.
    b. 4500-NH3 C-2021, Titration Method. The titrimetric method is 
used only on samples that have been carried through preliminary 
distillation. Ammonia is titrated with a standardized sulfuric acid 
titrant using a mixed indicator of methyl red and methylene blue. The 
2011 editorial revision currently is approved in Table IB for 
determination of ammonia as well as for determination of total Kjeldahl 
nitrogen after appropriate digestion/distillation of the sample.
    c. 4500-NH3 D-2021, Electrode Method. The ammonia-selective 
electrode uses a hydrophobic gas-permeable membrane to separate the 
sample solution from an electrode internal solution of ammonium 
chloride. Dissolved ammonia (NH3(aq) and 
NH4+) is converted to NH3(aq) by 
raising the pH to above 11 with a strong base. NH3(aq) 
diffuses through the membrane and changes the internal solution pH that 
is sensed by a pH electrode. The fixed level of chloride in the 
internal solution is sensed by a chloride ion-selective electrode that 
serves as the reference electrode of the sample. Potentiometric 
measurements are made with a pH meter having an expanded millivolt 
scale or with a specific ion meter. The 2011 editorial revision 
currently is approved in Table IB for determination of ammonia, as well 
as for determination of total Kjeldahl nitrogen after appropriate 
digestion/distillation of the sample.
    d. 4500-NH3 E-2021, Electrode Method. Ammonia is determined using 
an ammonia-selective electrode. When a linear relationship exists 
between concentration and response, known addition is convenient for 
measuring occasional samples because no calibration is needed. Because 
an accurate measurement requires that the concentration at least double 
as a result of the addition, sample concentration must be known within 
a factor of three. The total concentration of ammonia can be measured 
in the absence of complexing agents down to 0.8 mg/L NH3-N 
or in the presence of a large excess (50 to 100 times) of complexing 
agent. The 2011 editorial revision currently is approved in Table IB 
for determination of ammonia, as well as for determination of total 
Kjeldahl nitrogen after appropriate digestion/distillation of the 
sample.
    e. 4500-NH3 F-2021, Phenate Method. An intensely blue compound, 
indophenol, is formed by the reaction of ammonia, hypochlorite, and 
phenol catalyzed by sodium nitroprusside. The color is measured 
spectrophotometrically at 640 nm. The 2011 editorial revision currently 
is approved in Table IB for determination of ammonia, as well as for 
determination of total Kjeldahl nitrogen after appropriate digestion/
distillation of the sample.
    f. 4500-NH3 G-2021, Semi-Automated Phenate Method. Alkaline phenol 
and hypochlorite react with ammonia to form indophenol blue that is 
proportional to the ammonia concentration. The blue color formed is 
intensified with sodium nitroprusside. The color is measured 
spectrophotometrically at 630 to 660 nm. The 2011 editorial revision 
currently is approved in Table IB for determination of ammonia, as well 
as for determination of total Kjeldahl nitrogen after appropriate 
digestion/distillation of the sample.
    g. 4500-NH3 H-2021, Semi-Automated Phenate Method. A water sample 
containing ammonia or ammonium cation is injected into an FIA carrier 
stream to which a complexing buffer (alkaline phenol) and hypochlorite 
are added. This reaction, the Berthelot reaction, produces the blue 
indophenol dye. The blue color is intensified by the addition of 
nitroferricyanide. The resulting peak's absorbance is measured at 630 
nm. The peak area is proportional to the concentration of ammonia in 
the original sample. The 2011 editorial revision currently is approved 
in Table IB for determination of ammonia, as well as for determination 
of total Kjeldahl nitrogen after appropriate digestion/distillation of 
the sample.
    23. 4500-NO2- Nitrite as Nitrogen. 4500-NO2- 
B-2021, Spectrophotometric Method. Nitrite (NO2-) 
in a sample is determined through formation of a reddish-purple azo dye 
produced at pH 2.0 to 2.5 by coupling diazotized sulfanilamide with N-
(1-naphthyl)-ethylenediamine dihydrochloride (NED) and absorbance is 
measured spectrophotometrically at 543 nm. The 2011 editorial revision 
currently is approved in Table IB for determination of nitrite.
    24. 4500-NO3- Nitrogen (Nitrite/Nitrate as Nitrogen Series).
    a. 4500-NO3- D-2019, Nitrate Electrode Method. Nitrate is measured 
using an ion-selective electrode that develops a potential across a 
thin, inert membrane holding in place a water-immiscible liquid ion 
exchanger. The 2016 version of the method currently is approved in 
Table IB for determination of nitrate.
    b. 4500-NO3- E-2019, Cadmium Reduction Method. Nitrate 
(NO3-) is reduced almost quantitatively to 
nitrite (NO2-) in the presence of cadmium (Cd). 
This method uses commercially available Cd granules treated with copper 
sulfate (CuSO4) and packed in a glass column. The 
NO2- is then diazotized with sulfanilamide and 
coupled with NED to form a highly colored azo dye that is measured 
spectrophotometrically. To correct for any NO2- 
present in the sample before NO3- reduction, 
samples also must be analyzed without the reduction step. The 2016 
version of the method currently is approved in Table IB for 
determination of nitrate (by subtraction), as well as for determination 
of combined nitrate + nitrite, and for determination of nitrite singly 
when bypassing the reduction step.
    c. 4500-NO3- F-2019, Automated Cadmium Reduction Method. This is an 
automated version of the cadmium reduction method 4500 
NO3- E. Nitrate in a sample is reduced to nitrite 
using cadmium reduction and then diazotized with sulfanilamide and 
coupled with NED to form a highly colored azo dye that is measured 
spectrophotometrically. To correct for any NO2- 
present in the sample before NO3- reduction, 
samples also must be analyzed without the reduction step. The 2016 
version of the method currently is approved in Table IB for 
determination of nitrate (by subtraction), as well as for determination 
of combined nitrate +

[[Page 10734]]

nitrite, and for determination of nitrite singly when bypassing the 
reduction step.
    d. 4500-NO3- H-2019, Automated Hydrazine Reduction Method. Nitrate 
in a sample is reduced to nitrite using hydrazine sulfate then 
diazotized with sulfanilamide and coupled with NED to form a highly 
colored azo dye that is measured spectrophotometrically. The 2016 
version of the method currently is approved in Table IB for 
determination of combined nitrate and nitrite.
    e. 4500-NO3- I-2019, Cadmium Reduction Flow Injection Method. A 
sample is passed through a copperized cadmium column to quantitatively 
reduce its nitrate content to nitrite. The nitrite is diazotized with 
sulfanilamide and coupled with NED to yield a water-soluble dye with a 
magenta color whose absorbance at 540 nm is proportional to the nitrate 
+ nitrite in the sample. Nitrite concentrations may be determined by 
bypassing the cadmium column and nitrate concentration may be 
calculated by subtraction of the result for the nitrite concentration 
from the result for the combined nitrate + nitrite concentration. The 
2016 version of the method currently is approved in Table IB for 
determination of nitrate, as well as for determination of combined 
nitrate + nitrite, and for determination of nitrite singly by bypassing 
the reduction step.
    25. 4500-O Oxygen (Dissolved) Series.
    a. 4500-O B-2021, Iodometric Methods. A divalent manganese solution 
is added and then a strong alkali is added to a sample in a glass-
stoppered bottle and dissolved oxygen (DO) rapidly oxidizes an 
equivalent amount of the dispersed divalent manganous hydroxide 
precipitate into higher-valency hydroxides. Oxidized manganese reverts 
to the divalent state in the presence of iodide ions in an acidic 
solution, liberating an amount of iodine equivalent to the original DO 
content. The iodine is then titrated with a standard thiosulfate 
solution. The 2016 version of the method currently is approved in Table 
IB for determination of dissolved oxygen.
    b. 4500-O C-2021, Azide Modification. The sample is treated with 
manganous sulfate, potassium hydroxide, and potassium iodide (the 
latter two reagents combined in one solution) and finally sulfuric 
acid. The initial precipitate of manganous hydroxide, 
Mn(OH)2, combines with the dissolved oxygen in the sample to 
form a brown precipitate, manganic hydroxide, MnO(OH)2. Upon 
acidification, the manganic hydroxide forms manganic sulfate, which 
acts as an oxidizing agent to release free iodine from the potassium 
iodide. The iodine, which is stoichiometrically equivalent to the 
dissolved oxygen in the sample, is then titrated with sodium 
thiosulfate or phenylarsine oxide (PAO). The azide modification 
effectively removes nitrite interference, which is the most common 
interference in biologically treated effluents and incubated 
biochemical oxygen demand (BOD) samples. The 2016 version of the method 
currently is approved in Table IB for determination of dissolved 
oxygen.
    c. 4500-O D-2021, Permanganate Modification. The permanganate 
modification is used only on samples containing Fe(II) (e.g., acid mine 
water). Concentrated sulfuric acid, potassium permanganate in solution 
and potassium fluoride in solution are added to the sample. Enough 
KMnO4 solution is added to obtain a violet tinge that 
persists for 5 minutes. 0.5 to 1.0 mL potassium oxalate solution is 
then added only until permanganate color is removed completely. From 
this point, the procedure closely parallels that in 4500-O C. The 2016 
version of the method currently is approved in Table IB for 
determination of dissolved oxygen.
    d. 4500-O E-2021, Alum Flocculation Modification. Samples high in 
suspended solids may consume appreciable quantities of iodine in acid 
solution. The interference due to solids may be removed by alum 
flocculation. Concentrated ammonium hydroxide and aluminum potassium 
sulfate solution are added to a sample. The sample is allowed to settle 
for about 10 min and the clear supernatant is siphoned into a 250- to 
300-mL DO bottle until it overflows. From this point, the procedure 
closely parallels that in 4500-O C. The 2016 version of the method 
currently is approved in Table IB for determination of dissolved 
oxygen.
    e. 4500-O F-2021, Copper Sulfate-Sulfamic Acid Flocculation 
Modification. This modification is used for biological flocs (e.g., 
activated sludge mixtures), which have high oxygen utilization rates. A 
copper sulfate-sulfamic acid inhibitor solution is added to the sample. 
The suspended solids are allowed to settle, and the relatively clear 
supernatant liquor is siphoned into a 250- to 300-mL DO bottle. From 
this point, the procedure closely parallels that in 4500-O C. The 2016 
version of the method currently is approved in Table IB for 
determination of dissolved oxygen.
    f. 4500-O G-2021, Electrode Method. Oxygen-sensitive polarographic 
or galvanic membrane electrodes are composed of two solid metal 
electrodes in contact with supporting electrolyte separated from the 
test solution by a selective membrane. Polyethylene and fluorocarbon 
membranes are commonly used because they are permeable to molecular 
oxygen and are relatively rugged. The diffusion current is linearly 
proportional to the molecular-oxygen concentration. The measured 
current can be converted easily to concentration units (e.g., mg/L) by 
a number of calibration procedures. The 2016 version of the method 
currently is approved in Table IB for determination of dissolved 
oxygen.
    g. 4500-O H-2021, Luminescence-based Method. The optical probe uses 
luminescence-based oxygen sensors to measure the light-emission 
characteristics of a luminescent reaction; oxygen quantitatively 
quenches the luminescence. The change in the luminescence signal's 
lifetime correlates to the DO concentration. The 2016 version of the 
method currently is approved in Table IB for determination of dissolved 
oxygen.
    26. 4500-P Phosphorus Total and Ortho Phosphorus Series.
    a. 4500-P B-2021, Digestion Sample Preparation. Because phosphorus 
may occur in combination with organic matter, a digestion method to 
determine total phosphorus must be able to oxidize organic matter 
effectively to release phosphorus as orthophosphate. Three digestion 
methods are given in 4500-P B.3, 4, and 5. The perchloric acid method 
in B.5 is the most vigorous and time-consuming method, and is 
recommended for particularly difficult samples, such as sediments. The 
nitric acid-sulfuric acid method is recommended for most samples. The 
simplest digestion method that may be used for determination of total 
phosphorus is the persulfate oxidation technique in which 50 mL of an 
unfiltered sample is boiled with sulfuric acid and either ammonium 
persulfate or potassium persulfate for approximately 30-40 minutes or 
until a final volume of about 10 mL is reached. The 2011 editorial 
revision is currently approved in Table IB for preliminary treatment of 
samples to be used for determination of total phosphorus as 
orthophosphorus using manual or automated versions of the ascorbic acid 
reduction, colorimetric methods.
    b. 4500-P E-2021, Manual Method. Ammonium molybdate and antimony 
potassium tartrate react in an acid medium with orthophosphate to form 
phosphomolybdic acid, a heteropoly acid that is reduced to intensely 
colored molybdenum blue by ascorbic acid and is measured 
spectrophotometrically. This revision adds that possible interference 
from silicate should be

[[Page 10735]]

evaluated when reporting concentrations less than 10 [micro]g/L. The 
2011 editorial revision currently is approved in Table IB for 
determination of total phosphorus after digestion of the sample, as 
well as for determination of orthophosphorus in a filtered, undigested 
sample.
    c. 4500-P F-2021, Automated Ascorbic Acid Reduction Method. 
Ammonium molybdate and antimony potassium tartrate react with 
orthophosphate in an acid medium to form an antimony-phosphomolybdate 
complex, which on reduction with ascorbic acid yields an intense blue 
color suitable for photometric measurement using continuous flow 
analytical equipment. The 2011 editorial revision currently is approved 
in Table IB for determination of total phosphorus after digestion of 
the sample, as well as for determination of orthophosphorus in a 
filtered, undigested sample.
    d. 4500-P G-2021, Automated. Ammonium molybdate and antimony 
potassium tartrate react with orthophosphate in an acid medium to form 
an antimony-phosphomolybdate complex, which on reduction with ascorbic 
acid yields an intense blue color suitable for photometric measurement 
using flow injection analysis. The 2011 editorial revision currently is 
approved in Table IB for determination of total phosphorus after 
digestion of the sample as well, as for determination of 
orthophosphorus in a filtered, undigested sample.
    e. 4500-P H-2021, Automated Total Phosphorus. Samples are manually 
digested using the approved procedure for preliminary treatment of 
samples to be used for determination of total phosphorus. When the 
resulting solution is injected onto the manifold, the orthophosphate 
ion reacts with ammonium molybdate and antimony potassium tartrate 
under acidic conditions to form a complex. This complex is reduced with 
ascorbic acid to form a blue complex suitable for photometric 
measurement using flow injection analysis. The 2011 editorial revision 
currently is approved in Table IB for determination of total 
phosphorus.
    27. 4500-S2- Sulfide Series.
    a. 4500-S2- B-2021, Sample Pretreatment. Dissolved 
sulfide is measured by first removing insoluble matter. This is done by 
adding sodium hydroxide and aluminum chloride solutions producing an 
aluminum hydroxide floc that is settled, leaving a clear supernatant 
for analysis. The 2011 editorial revision currently is approved in 
Table IB for preliminary treatment of samples to be used for 
determination of sulfide.
    b. 4500-S2- C-2021, Sample Pretreatment. Interferences 
due to sulfite, thiosulfate, iodide, and many other soluble substances, 
but not ferrocyanide, are eliminated by first precipitating zinc 
sulfide (ZnS) by addition of sodium hydroxide and zinc acetate 
solutions, removing the supernatant, and replacing it with reagent 
water. The same procedure is used even when not needed for removal of 
interferences, to concentrate sulfide prior to analysis. The 2011 
editorial revision currently is approved in Table IB for preliminary 
treatment of samples to be used for determination of sulfide.
    c. 4500-S2- D-2021, Colorimetric Method. The methylene 
blue method is based on the reaction of sulfide, ferric chloride, and 
dimethyl-p-phenylenediamine to produce methylene blue. Ammonium 
phosphate is added after color development to remove ferric chloride 
color, which is measured photometrically. The procedure is applicable 
at sulfide concentrations between 0.1 and 20.0 mg/L. There are no other 
procedural changes. The 2011 editorial revision currently is approved 
in Table IB for determination of sulfide.
    d. 4500-S2- F-2021, Titrimetric. Iodine oxidizes sulfide 
in acid solution. A titration based on this reaction is an accurate 
method for determining sulfide at concentrations above 1 mg/L if 
interferences are absent and if loss of H2S is avoided. The 
2011 editorial revision currently is approved in Table IB for 
determination of sulfide.
    e. 4500-S2- G-2021, Ion-Selective Electrode Method. The 
potential of a sulfide ion-selective electrode (ISE) is related to the 
sulfide ion activity. An alkaline antioxidant reagent (AAR) is added to 
samples and standards to inhibit oxidation of sulfide by oxygen and to 
provide a constant ionic strength and pH. Use of the AAR allows 
calibration in terms of total dissolved sulfide concentration. All 
samples and standards must be at the same temperature. Sulfide 
concentrations between 0.032 mg/L and 100 mg/L can be measured without 
preconcentration. For lower concentrations, preconcentration is 
necessary. The 2011 editorial revision currently is approved in Table 
IB for determination of sulfide.
    28. 4500-SiO2 Silica Series.
    a. 4500-SiO2 C-2021, Colorimetric Method. Ammonium molybdate at pH 
approximately 1.2 reacts with silica and any phosphate present to 
produce heteropoly acids. Oxalic acid is added to destroy the 
molybdophosphoric acid, but not the molybdosilicic acid. Even if 
phosphate is known to be absent, the addition of oxalic acid is highly 
desirable and is a mandatory step. The intensity of the yellow color 
produced is proportional to the concentration of molybdate-reactive 
silica and is measured photometrically. The 2011 editorial revision 
currently is approved in Table IB for determination of silica.
    b. 4500-SiO2 E-2021, Automated Method for Molybdate-Reactive 
Silica. Ammonium molybdate at pH approximately 1.2 reacts with silica 
and any phosphate present to produce heteropoly acids. Oxalic acid is 
added to destroy the molybdophosphoric acid, but not the molybdosilicic 
acid. The yellow molybdosilicic acid is reduced by means of amino 
naphthol sulfonic acid to heteropoly blue. The blue color is more 
intense than the yellow color of 4500-SiO2 C and provides 
increased sensitivity. The 2011 editorial revision currently is 
approved in Table IB for determination of silica.
    c. 4500-SiO2 F-2021, Automated Method for Molybdate-Reactive 
Silicate. Silicate reacts with molybdate under acidic conditions to 
form yellow beta-molybdosilicic acid. This acid is subsequently reduced 
with stannous chloride to form a heteropoly blue complex that is 
measured photometrically. Oxalic acid is added to reduce the 
interference from phosphate. The 2011 editorial revision currently is 
approved in Table IB for determination of silica.
    29. 4500-SO42-Sulfate Series.
    a. 4500-SO42-C-2021, Gravimetric Method with Ignition of Residue. 
Sulfate is precipitated in a hydrochloric acid (HCl) solution as barium 
sulfate (BaSO4) by the addition of barium chloride 
(BaCl2). The precipitation is carried out near the boiling 
temperature, and after a period of digestion, the precipitate is 
filtered, washed with water until free of Cl-, ignited at 
800 [deg]C for an hour and weighed as BaSO4. The 2011 
editorial revision currently is approved in Table IB for determination 
of sulfate.
    b. 4500-SO42-D-2021, Gravimetric Method with Drying of Residue. 
Sulfate is precipitated in a hydrochloric acid (HCl) solution as barium 
sulfate (BaSO4) by the addition of barium chloride 
(BaCl2). The precipitation is carried out near the boiling 
temperature, and after a period of digestion the precipitate is 
filtered, washed with water until free of Cl-, dried to a 
constant weight in an oven at 105 [deg]C or higher, and weighed as 
BaSO4. The 2011 editorial revision currently is approved in 
Table IB for determination of sulfate.
    c. 4500-SO42-E-2021, Turbidimetric Method. Sulfate ion 
(SO42-) is precipitated in an acetic acid medium

[[Page 10736]]

with barium chloride (BaCl2) to form barium sulfate 
(BaSO4) crystals of uniform size. Light absorbance of the 
BaSO4 suspension is measured by a photometer and the 
SO42- concentration is determined by comparison 
of the reading with a standard curve. The 2011 editorial revision 
currently is approved in Table IB for determination of sulfate.
    d. 4500-SO42-F-2021, Automated Colorimetric Method. Barium sulfate 
is formed by the reaction of the SO42- with 
barium chloride (BaCl2) at a low pH. At high pH, excess 
barium reacts with methylthymol blue (MTB) to produce a blue chelate. 
The uncomplexed methylthymol blue is gray. The intensity of gray 
(uncomplexed methylthymol blue) is measured photometrically and is 
proportional to concentration of sulfate. The 2011 editorial revision 
currently is approved in Table IB for determination of sulfate.
    e. 4500-SO42-G-2021, Automated Colorimetric Method. At pH 13.0, 
barium forms a blue complex with MTB. The sample is injected into a 
low, but known, concentration of sulfate. The sulfate from the sample 
then reacts with the ethanolic barium-MTB solution and displaces the 
MTB from the barium to give barium sulfate and uncomplexed MTB. 
Uncomplexed MTB has a grayish color. The pH is raised with NaOH and the 
gray color of the uncomplexed MTB is measured photometrically. The 
intensity of the gray color is proportional to the sulfate 
concentration. The 2011 editorial revision currently is approved in 
Table IB for determination of sulfate.
    30. Sulfite 4500-SO32-B-2021, Titrimetric Iodometric Method. An 
acidified sample containing sulfite (SO32-) is 
titrated with a standardized potassium iodide-iodate titrant. Free 
iodine, liberated by the iodide-iodate reagent, reacts with 
SO32-. The titration endpoint is signaled by the 
blue color resulting from the first excess of iodine reacting with a 
starch indicator. The 2011 editorial revision currently is approved in 
Table IB for determination of sulfite.
    31. 5520 Oil and Grease Series.
    a. 5520 B-2021, Liquid-Liquid, Partition-Gravimetric Method. 
Dissolved or emulsified oil and grease is extracted from water by 
intimate contact with an extracting solvent (n-hexane). The extract is 
dried over sodium sulfate. The solvent is then distilled from the 
extract and the hexane extractable material is desiccated and weighed. 
Some extractables, especially unsaturated fats and fatty acids, oxidize 
readily; hence, special precautions regarding temperature and solvent 
vapor displacement are included to minimize this effect. Organic 
solvents shaken with some samples may form an emulsion that is very 
difficult to break. This method includes a means for handling such 
emulsions. Recovery of solvents is discussed. Solvent recovery can 
reduce both vapor emissions to the atmosphere and costs. The 2011 
editorial revision currently is approved in Table IB for determination 
of oil and grease (hexane extractable material or HEM).
    b. 5520 F-2021, Hydrocarbons. The oil and grease extracted by 5520 
B is used for this test. When only hydrocarbons are of interest, this 
procedure is introduced before final measurement. When hydrocarbons are 
to be determined after total oil and grease has been measured, 
redissolve the extracted oil and grease in n-hexane. Silica gel has the 
ability to adsorb polar materials. The solution of extracted 
hydrocarbons and fatty materials in n-hexane is mixed with silica gel, 
and the fatty acids are removed selectively from solution. The solution 
is filtered to remove the silica gel, the solvent is distilled, and the 
silica gel treated hexane extractable material (SGT-HEM) is weighed. 
The materials not eliminated by silica gel adsorption are designated 
hydrocarbons by this test. The 2011 editorial revision currently is 
approved in Table IB for determination of oil and grease (hexane 
extractable material or HEM).
    32. 5530 Phenols Series.
    a. 5530 B-2021, Manual Distillation. Phenols, defined as hydroxy 
derivatives of benzene and its condensed nuclei, may occur in domestic 
and industrial wastewaters, natural waters, and potable water supplies. 
Phenols are distilled from nonvolatile impurities. Because the 
volatilization of phenols is gradual, the distillate volume must 
ultimately equal that of the original sample. The 2010 version of the 
method currently is approved in Table IB for preliminary treatment of 
samples to be used for determination of phenols.
    b. 5530 D-2021, Colorimetric Method. Steam-distillable phenolic 
compounds react with 4-aminoantipyrine at pH 7.9  0.1 in 
the presence of potassium ferricyanide to form a colored antipyrine 
dye. This dye is kept in aqueous solution and the absorbance is 
measured photometrically at 500 nm. The 2010 version of the method 
currently is approved in Table IB for determination of phenol. Note 
that for regulatory compliance monitoring required under the Clean 
Water Act, the colorimetric reaction must be performed at a pH of 10.0 
 0.2 as stated in 40 CFR 136.3, Table IB, footnote 27.
    33. 5540 Surfactants.
    5540 C-2021. This colorimetric method comprises three successive 
extractions from an acid aqueous medium containing excess methylene 
blue into chloroform (CHCl3), followed by an aqueous 
backwash and measurement of the blue color in the CHCl3 by 
spectrophotometry at 652 nm. The method is applicable at methylene blue 
active substances concentrations down to about 0.025 mg/L. The 2011 
editorial revision currently is approved in Table IB for determination 
of surfactants.
    34. 6200 Volatile Organic Compounds Series.
    a. In the 6200 B-2020, Purge and Trap Capillary-Column Gas 
Chromatographic/Mass Spectrometric (GC/MS) Method, volatile organic 
compounds are transferred efficiently from the aqueous to the gaseous 
phase by bubbling an inert gas (e.g., helium) through a water sample 
contained in a specially designed purging chamber at ambient 
temperature. The vapor is swept through a sorbent trap that adsorbs the 
analytes of interest. After purging is complete, the trap is heated and 
back-flushed with the same inert gas to desorb the compounds onto a gas 
chromatographic column. The gas chromatograph is temperature-programmed 
to separate the compounds. The detector is a mass spectrometer. The 
2011 editorial revision currently is approved in Table IC for 
determination of benzene, bromodichloromethane, bromoform, 
bromomethane, carbon tetrachloride, chlorobenzene, chloroethane, 
chloroform, chloromethane, dibromochloromethane, 1,2-dichlorobenzene, 
1,3-dichlorobenzene, 1,4-dichlorobenzene, dichlorodifluoromethane, 1,1-
dichloroethane, 1,2-dichloroethane, 1,1-dichloroethene, trans-1,2-
dichloroethene, 1,2-dichloropropane, cis-1,3-dichloropropene, trans-
1,3-dichloropropene, ethylbenzene, methylene chloride, 1,1,2,2-
tetrachloroethane, tetrachloroethene, toluene, 1,1,1-trichloroethane, 
1,1,2-trichloroethane, trichloroethene, trichlorofluoromethane, and 
vinyl chloride.
    b. 6200 C-2020, Purge and Trap Capillary-Column Gas Chromatographic 
(GC) Method. Volatile organic compounds are transferred efficiently 
from the aqueous to the gaseous phase by bubbling an inert gas (e.g., 
helium) through a water sample contained in a specially designed 
purging chamber at ambient temperature. The vapor is swept through a 
sorbent trap that adsorbs the analytes of interest. After

[[Page 10737]]

purging is complete, the trap is heated and back-flushed with the same 
inert gas to desorb the compounds onto a gas chromatographic column. 
The gas chromatograph is temperature-programmed to separate the 
compounds and detected using a photoionization detection and an 
electrolytic conductivity detection in series. The 2011 editorial 
revision currently is approved in Table IC for determination of 
benzene, bromodichloromethane, bromoform, bromomethane, carbon 
tetrachloride, chlorobenzene, chloroethane, chloroform, chloromethane, 
dibromochloromethane, 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-
dichlorobenzene, 1,1-dichloroethane, 1,2-dichloroethane, 1,1-
dichloroethene, trans-1,2-dichloroethene, 1,2-dichloropropane, cis-1,3-
dichloropropene, trans-1,3-dichloropropene, ethylbenzene, methylene 
chloride, 1,1,2,2-tetrachloroethane, tetrachloroethene, toluene, 1,1,1-
trichloroethane, 1,1,2-trichloroethane, trichloroethene, 
trichlorofluoromethane, and vinyl chloride.
    35. 6410 Extractable Base/Neutrals and Acids.
    6410 B-2020, Liquid-Liquid Extraction Gas Chromatographic/Mass 
Spectrometric Method. This method is applicable to the determination of 
organic compounds that are partitioned into an organic solvent and are 
amenable to gas chromatography in municipal and industrial discharges. 
A measured volume of sample is extracted serially with methylene 
chloride at a pH of approximately 2 and again at pH 11. The extract is 
dried, concentrated, and analyzed by GC/MS. Qualitative compound 
identification is based on retention time and relative abundance of 
three characteristic masses (m/z). Quantitative analysis uses internal-
standard techniques with a single characteristic m/z. This revision 
adds a note that although the method was validated extracting base 
neutrals first and then acids, performance may be improved by 
extracting acids first and then base neutrals. In addition, EPA 
proposes to approve method 6410-B for endrin aldehyde in Table ID. This 
parameter was inadvertently left off the 2000 MUR rulemaking. The 2000 
version of the method currently is approved in Table IC for 
determination of acenaphthene, acenaphthylene, anthracene, benzidine, 
benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, 
benzo(g,h,i)perylene, benzo(k)fluoranthene, butyl benzyl phthalate, 
bis(2-chloroethoxy) methane, bis(2-chloroethyl) ether, bis(2-
ethylhexyl) phthalate, bromodichloromethane, 4-bromophenyl phenyl 
ether, 4-chloro-3-methyl phenol, 2-chloronaphthalene, 2-chlorophenol, 
4-chlorophenyl phenyl ether, chrysene, dibenzo(a,h)anthracene, 3,3'-
dichlorobenzidine, 2,4-dichlorophenol, diethyl phthalate, 2,4-
dimethylphenol, dimethyl phthalate, di-n-butyl phthalate, di-n-octyl 
phthalate, 2,4-dinitrophenol, 2,4-dinitrotoluene, 2,6-dinitrotoluene, 
fluoranthene, fluorene, hexachlorobenzene, hexachlorobutadiene, 
hexachlorocyclopentadiene, indeno(1,2,3-c,d) pyrene, isophorone, 2-
methyl-4,6-dinitrophenol, naphthalene, nitrobenzene, 2-nitrophenol, 4-
nitrophenol, n-nitrosodi-n-propylamine, n-nitrosodiphenylamine, PCB-
1016, PCB-1221, PCB-1232, PCB-1242, PCB-1248, PCB-1254, PCB-1260, 
pentachlorophenol, phenanthrene, phenol, pyrene, 1,2,4-
trichlorobenzene, and 2,4,6-trichlorophenol and in Table ID for 
determination of aldrin, [alpha]-BHC, [beta]-BHC, [delta]-BHC, [gamma]-
BHC (lindane), chlordane, 4,4'-DDD, 4,4'-DDE, 4,4'-DDT, dieldrin, 
endosulfan I, endosulfan II, endosulfan sulfate, endrin, heptachlor, 
heptachlor epoxide, and toxaphene.
    36. 6420 Phenols.
    6420 B-2020, Liquid-Liquid Extraction Gas Chromatographic Method. A 
measured volume of sample is acidified and extracted with methylene 
chloride. The extract is dried and exchanged to 2-propanol during 
concentration. Target analytes in the extract are separated by gas 
chromatography and are identified by retention time and measured with a 
flame ionization detector, or derivatized and measured with an electron 
capture detector. This revision of the method replaces distilled, 
deionized water with reagent water, adds that the packed columns used 
for validation of the method are no longer available or recommended, 
and includes information on alternative capillary columns that may be 
used. The 2000 version of the method currently is approved in Table IC 
for determination of 4-chloro-3-methylphenol, 2-chlorophenol, 2,4-
dichlorophenol, 2,4-dimethylphenol, 2,4-dinitrophenol, 2-methyl-4,6-
dinitrophenol, 2-nitrophenol, 4-nitrophenol, pentachlorophenol, phenol, 
and 2,4,6-trichlorophenol.
    37. 6440 Polynuclear Aromatic Hydrocarbons.
    6440 B-2021, Liquid-Liquid Extraction Chromatographic Method. A 
measured volume of sample is extracted with methylene chloride. The 
extract is dried, concentrated, and separated by the high-performance 
liquid chromatographic (HPLC) or gas chromatographic (GC) method. 
Ultraviolet (UV) and fluorescence detectors are used with HPLC to 
identify and measure the polynuclear aromatic hydrocarbons. A flame 
ionization detector is used with GC. The 2005 version of the method 
currently is approved in Table IC for determination of acenaphthene, 
acenaphthylene, anthracene, benzo(a)anthracene, benzo(a)pyrene, 
benzo(b)fluoranthene, benzo(g,h,i)perylene, benzo(k)fluoranthene, 
chrysene, dibenzo(a,h)anthracene, fluoranthene, fluorene, indeno(1,2,3-
c,d)pyrene, naphthalene, phenanthrene, and pyrene.
    38. 6630 Organochlorine Pesticides Series.
    a. 6630 B-2021, Liquid-Liquid Extraction Gas Chromatographic Method 
I, in this procedure, the pesticides are extracted with a mixed 
solvent, diethyl ether-hexane or methylene chloride-hexane, by either 
liquid-liquid extraction using a separatory funnel or by continuous 
liquid-liquid extraction. The extract is concentrated by evaporation 
and, if necessary, is cleaned up by column adsorption chromatography. 
The individual pesticides then are separated by gas chromatography and 
the compounds are measured with an electron capture detector (ECD). 
This revision of the method adds information regarding alternative 
capillary columns that may be used in place of the packed columns that 
were used for validation of the method, removes information regarding 
preparation of packed columns, replaces information regarding manual 
injection technique with use of an autosampler and states that gas 
chromatography/mass spectrometry (GC/MS) may be used for confirmatory 
analyses in place of a second column and ECD detection. There are no 
other procedural changes. The 2007 version of the method currently is 
approved in Table ID for determination of aldrin, [alpha]-BHC, [beta]-
BHC, [delta]-BHC, [gamma]-BHC (lindane), captan, carbophenothion, 
chlordane, 4,4'-DDD, 4,4'-DDE, 4,4'-DDT, dichloran, dieldrin, 
endosulfan I, endosulfan II, endrin, heptachlor, heptachlor epoxide, 
isodrin, malathion, methoxychlor, mirex, parathion methyl, parathion 
ethyl, PCNB, strobane, toxaphene, and trifluralin.
    b. In 6630 C-2021, Liquid-Liquid Extraction Gas Chromatographic 
Method II, a measured volume of sample is extracted with methylene 
chloride either by liquid-liquid extraction using separatory funnels or 
by continuous liquid-liquid extraction. The extract is dried and 
exchanged to

[[Page 10738]]

hexane during concentration. The target analytes are separated by gas 
chromatography and the compounds are measured with an electron capture 
detector (ECD). This revision of the method adds information regarding 
alternative capillary columns that may be used in place of the packed 
columns that were used for validation of the method, and states that 
gas chromatography/mass spectrometry (GC/MS) may be used for 
confirmatory analyses in place of a second column and ECD detection. 
There are no other procedural changes. The 2007 version of the method 
currently is approved in Table ID for determination of aldrin, [alpha]-
BHC, [beta]-BHC, [delta]-BHC, [gamma]-BHC (lindane), chlordane, 4,4'-
DDD, 4,4'-DDE, 4,4'-DDT, dieldrin, endosulfan I, endosulfan II, 
endosulfan sulfate, endrin, endrin aldehyde, heptachlor, heptachlor 
epoxide, isodrin, methoxychlor, mirex, PCNB, strobane, and toxaphene.
    39. 6640 Acidic Herbicide Compounds.
    6640 B-2021, Micro Liquid-Liquid Extraction Gas Chromatographic 
Method. A 40-mL sample is adjusted to pH >=12 with 4 N sodium hydroxide 
and is kept for 1 hour at room temperature to hydrolyze derivatives. 
Because the chlorphenoxy acid herbicides are formulated as a variety of 
esters and salts, the hydrolysis step is required and may not be 
skipped. The aqueous sample then is acidified with sulfuric acid to pH 
<=1 and extracted with 4 mL of methyl tert-butyl ether (MtBE) that 
contains the internal standard. The chlorinated acids, which have been 
partitioned into the MtBE, then are converted to methyl esters by 
derivatization with diazomethane. The target esters are separated and 
detected by capillary column gas chromatography using an electron 
capture detector (GC/ECD). Analytes are quantified using an internal-
standard-based calibration curve. The 2006 editorial revision currently 
is approved in Table IC for determination of 2,4-D, 2,4,5-T, and 2,4,5-
TP (Silvex).

D. Changes to 40 CFR 136.3 To Include Alternate Test Procedures in 
Table IC

    To promote method innovation, EPA maintains a program that allows 
method developers to apply for EPA review and potential approval of an 
alternative method to an existing approved method. This alternate test 
procedure (ATP) program is described for CWA applications at 40 CFR 
136.4 and 136.5. EPA is proposing two ATPs for nationwide use. Based on 
EPA's review, the performance of these ATPs is equally effective as 
other methods already approved for measurement of 2,3,7,8-substituted 
tetra- through octa-chlorinated dibenzo-p-dioxins and dibenzofurans 
(PCDDs/PCDFs) in wastewater. The ATP applicants supplied EPA with study 
reports that contain the data from their validation studies. These 
study reports, the final methods, and the letters documenting EPA's 
review are included as supporting documents in the docket for this 
proposed rule.
    These proposed new methods are: SGS AXYS Method ATM 16130, 
``Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated 
Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using Waters and 
Agilent Gas Chromatography-Tandem-Mass Spectrometry (GC/MS/MS), 
Revision 1.0 and Pace Analytical Method PAM-16130-SSI, ``Determination 
of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo-p-
Dioxins and Dibenzofurans (CDDs/CDFs) Using Shimadzu Gas Chromatography 
Mass Spectrometry (GC-MS/MS), Revision 1.1.'' These ATPs are the 
results of separate collaborative efforts between SGS AXYS Analytical 
Services Ltd, and the instrument manufacturers Waters Corporation, 
Agilent Technologies, and between Pace Analytical Services LLC and the 
instrument manufacturer Shimadzu Scientific Instruments, Inc. These 
final methods are heavily adapted from Method 1613B. Neither ATP makes 
changes to the extraction or cleanup procedures specified in Method 
1613B. All required quality control tests (or analogous tests) and 
associated QC acceptance criteria have been included in both SGS AXYS 
16130 and PAM-16130-SSI.
    To minimize costs to both the applicants and the Agency where 
possible, SGS AXYS, Pace Analytical, and the instrument manufacturers 
who collaborated on these methods worked closely with EPA's CWA ATP 
Coordinator to design single-laboratory validation studies for these 
methods. The goal of these validation studies was to demonstrate that 
all of the performance criteria specified in Method 1613B could be met 
and that comparable performance could be achieved when using GC-MS/MS 
instrumentation for determination of PCDDs/PCDFs in extracts from real-
world samples.
    EPA Method 1613B was promulgated at 40 CFR 136 in 1995 and remains 
the only approved method for dioxins and furans at NPDES permit levels 
(Methods 613 and 625.1 may only be used for screening). Method 1613B is 
also the only method approved at 40 CFR part 136 that relies on gas 
chromatography-high resolution mass spectrometry (GC/HRMS) as the 
determinative technique. As a result, the need for GC/HRMS instruments 
is somewhat limited, and market forces have led some instrument vendors 
to move away from supporting new GC/HRMS instrumentation. In addition, 
in the last 30 years, there has been substantial consolidation of 
manufacturers, with the disappearance of many of the vendors whose 
instruments were used to develop and validate Method 1613B.
    In these two methods, referred to in the rule as ATM 16130 and PAM 
16130-SSI, each sample is spiked with the same suite of carbon-13 
labeled standards prior to extraction and those standards are used for 
isotope dilution quantitation in the same way as is done in EPA Method 
1613B. All of the relevant QC acceptance criteria are the same in the 
methods as well. The difference between these methods and the approved 
EPA method is the use of an MS/MS detector system that uses Multiple 
Reaction Monitoring (MRM) in place of a high resolution mass 
spectrometer (HRMS) detector system. The GC portions of the methods did 
not change.

E. Corrections or Amendments to the Text and Tables of 40 CFR Part 136

    In addition to the method revisions discussed in Section II.C of 
this preamble, Standard Methods has revised certain of their general 
quality control sections (2020, 3020, 4020 and 5020). EPA is proposing 
to update the year of the current references to these sections in 136.3 
Table IB footnote 85, as well as add a reference to an additional 
Standard Methods Quality Control Section: Part 6000 Individual Organic 
Compounds, 6020, based on EPA's review of these sections. These Quality 
Control Standards are available for download at www.standardmethods.org 
at no charge. Further, during the preparation of this proposed 
rulemaking, EPA identified several minor errors or inconsistencies in 
the tables of approved methods. Therefore, EPA is proposing the 
following changes to 40 CFR 136.3, Tables IA, IB, IC or ID:
    1. Table IA. Removing the units of ``number per 100 mL'' under 
parameter 1. Coliform (fecal), because parameter 1 is specifically for 
biosolids that are reported as ``number per gram dry weight''.
    2. Table IA. Moving USGS Method ``B-0050-85'' from parameter 1. 
Coliform (fecal) number per gram dry weight to parameter 2. Coliform 
(fecal) number per 100 mL, to address an error from the previous 
rulemaking when Parameter 1 Coliform (fecal) was split

[[Page 10739]]

into two parameters to eliminate confusion as to which methods were 
approved for biosolids.
    3. Table IA. Moving the phrase ``two-step'' in parameter 3, in the 
``Method'' column from the second to the third line which returns the 
phrase to the proper line after having been inadvertently moved.
    4. Table IB. Revising footnote 85 to remove bullet formatting.
    5. Table IB. EPA proposes adding footnote 86 to Method 419D, listed 
as an approved method for determination nitrate using Colorimetric 
(Brucine sulfate) methodology. This addition corrects a long-standing 
typographical error regarding the appropriate footnote for this method 
in Table IB.
    6. Table IB. Correcting an inadvertent error to footnote 57. The 
reference number was incorrectly changed to 335.4-1. The correct number 
is 335.4.
    7. Tables IC and ID. Proposes adding footnote 15 to the Standard 
Method Column header and adding footnote 15 to refer to Quality Control 
Section: Part 6000 Individual Organic Compounds, 6020 (2019).
    8. Table IC. The parameter 39, dichlorodifluoromethane, should 
refer to Method 6200 B rather than 6200 C for the GC/MS method.
    9. Table IC. Parameters 66-72, 95, 96 and 97. These parameters are 
missing the footnote 10 that was inadvertently dropped in an earlier 
rulemaking. Footnote 10 to table IC applies to all of the 17 dioxin and 
furan congeners.
    10. Table IH. Parameter 2 has method B-0025-85 is moved down one 
row because it was inadvertently moved. This method is a one-step 
membrane filtration (MF) method rather than a most probable number 
(MPN) method.
    11. Footnote 5 to Table II for the preservation and holding time 
requirements for cyanide to add the year (2015) of the ASTM method 
D7365-09a (15). This practice is applicable for the collection and 
preservation of water samples for the analysis of cyanide. Samples are 
collected in appropriate containers and mitigated for known 
interferences either in the field during sample collection or in the 
laboratory prior to analysis. The sampling, preservation and mitigation 
of interference procedures described in this practice are recommended 
for the analysis of total cyanide, available cyanide, weak acid 
dissociable cyanide, and free cyanide by ASTM Methods D2036, D4282, 
D4374, D6888, D6994, D7237, D7284, and D7511.
    The recommended sampling and preservation procedures in the ASTM 
method have not changed since 2009, but the change to footnote 5 will 
simplify identification of the current method that is available from 
ASTM International. The 2015 reapproval date was already updated in 
footnote 6 to Table II in the 2021 methods update rule; however, adding 
the reapproval date was overlooked in the IBR section and in footnote 5 
to Table II.

F. Changes to 40 CFR 136.3 To Include New Standard Methods Committee 
Methods Based on Previously Approved Technologies

    EPA is proposing adding five new methods in furtherance of the 
National Technology Transfer and Advancement Act of 1995 (NTTAA), 
Public Law 104-113, that provides that Federal agencies and departments 
shall use technical standards developed or adopted by the VCSBs if 
compliance would not be inconsistent with applicable law or otherwise 
impracticable. These methods were submitted by Standard Methods and are 
consistent with other already approved methods. EPA is adding 4500-
CN- P-2021, 4500-CN- Q-2021, 4500 CN- 
R-2021, 4500-F- G-2021 to Table IB for cyanide and fluoride 
and is adding 5520 G-2021 to Table IB for oil and grease, based on the 
following reasons:
    1. Cyanide. Although method 4500-CN- P-2021, Total 
Cyanide by Segmented Flow Injection, UV-Irradiation with Gas Diffusion, 
and Amperometric Measurement is new to Standard Methods for the 
Examination of Water and Wastewater, it is based on ASTM D7511-12(17), 
which is approved in Table IB for determination of total cyanide and 
relies on the same underlying chemistry and determinative technique to 
determine total cyanide. Total cyanide consists of dissolved HCN, 
sodium cyanide (NaCN), and various metal-cyanide complexes, which a 
continuous flow analyzer converts to aqueous HCN by mixing it with 
sulfuric acid, irradiating with UV light, and precipitating potentially 
interfering sulfides with bismuth ion. The aqueous HCN is captured in a 
donor stream that is passed across a hydrophobic gas-permeable 
membrane, which selectively diffuses the gaseous HCN into a parallel 
acceptor stream of dilute sodium hydroxide forming dissolved 
CN-. The cyanide ion in this acceptor stream is measured 
using an amperometric detector, where the cyanide ion dissolves the 
silver electrode, resulting in a proportional current.
    2. 4500-CN- Q-2021, Weak and Dissociable Cyanide by Flow Injection, 
Gas Diffusion, and Amperometric Measurement. Weak and dissociable 
cyanide consists of dissolved HCN, NaCN, and various metal-cyanide 
complexes and includes the same forms of cyanide as those measured 
using other methods approved in Table IB for determination of available 
cyanide. Analysts pretreat for weak and dissociable cyanide by mixing a 
sample with ligand reagents. They then inject the sample into a 
sulfuric acid and bismuth nitrate solution to produce a donor stream 
containing aqueous dissolved HCN and precipitated sulfide, if sulfide 
is present. The donor stream is passed across a hydrophobic gas-
permeable membrane, which selectively diffuses gaseous HCN into a 
parallel acceptor stream of dilute sodium hydroxide, forming dissolved 
CN-. The cyanide ion in this acceptor stream is measured using an 
amperometric detector, where the cyanide ion dissolves the silver 
electrode, resulting in a proportional current. Although this method is 
new to Standard Methods for the Examination of Water and Wastewater, it 
is based on ASTM D6888-16, which is approved in Table IB for 
determination of available cyanide and relies on the same underlying 
chemistry and determinative technique to determine available cyanide.
    3. 4500-CN- R-2021, Free Cyanide by Flow Injection, Gas Diffusion, 
and Amperometric Measurement. Free cyanide (FCN) consists of dissolved 
HCN, NaCN, and the soluble fraction of various metal-cyanide complexes. 
To determine FCN, analysts pretreat a sample by mixing it with a 
buffered solution in the pH range of 6 to 8 that simulates the 
receiving water resulting in a donor stream containing aqueous 
dissolved HCN in equilibrium with the cyanide anion. The donor stream 
is passed across a hydrophobic gas-permeable membrane, which 
selectively diffuses gaseous HCN into a parallel acceptor stream that 
consists of dilute sodium hydroxide, forming dissolved CN-. The cyanide 
ions in this acceptor stream are measured when it is passed through an 
amperometric detector, where the cyanide ion dissolves the silver 
electrode, resulting in a proportional current. Although this method is 
new to Standard Methods for the Examination of Water and Wastewater, it 
is based on ASTM D7237-15, which is approved in Table IB for 
determination of free cyanide and relies on the same underlying 
chemistry and determinative technique to determine free cyanide.
    4. Fluoride. 4500-F- G-2021, Ion-Selective Electrode Flow Injection 
Analysis is an automated version of method 4500-F- C and 
relies on the same underlying chemistry and

[[Page 10740]]

determinative technique as USGS Method I-4237-85, which currently is 
approved in Table IB for determination of fluoride. Fluoride is 
determined potentiometrically by using a combination fluoride ion 
selective electrode (ISE) in a flow cell. The fluoride electrode 
consists of a lanthanum fluoride crystal across which a potential is 
developed by fluoride ions.
    5. Oil and Grease. In 5520 G-2021, Solid-Phase, Partition-
Gravimetric Method, dissolved or emulsified oil and grease is extracted 
from water by passing a sample through a solid-phase extraction (SPE) 
disk where the oil and grease are adsorbed by the disk and subsequently 
eluted with n-hexane. SPE is a modification allowed under EPA Methods 
1664 A and B and relies on the same underlying chemistry and 
determinative technique as Methods 1664 A and B. Some extractables, 
especially unsaturated fats and fatty acids, oxidize readily; hence, 
special precautions regarding temperature and solvent vapor 
displacement are provided. This method is not applicable to materials 
that volatilize at temperatures below 85 [deg]C, or crude and heavy 
fuel oils containing a significant percentage of material not soluble 
in n-hexane. This method may be a satisfactory alternative to liquid-
liquid extraction techniques, especially for samples that tend to form 
difficult emulsions during the extraction step.

IV. Incorporation 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 parameter (or 
pollutant) and regulated entities often have a choice in selecting a 
method. The proposed rule contains revisions to VCSB methods that are 
currently incorporated by reference (see Sections III.B, III.C, and 
III.F of this preamble). Two VCSBs have made such revisions, Standard 
Methods and ASTM. The proposed VCSB methods are consistent with the 
requirements of the National Technology Transfer and Advancement Act 
(NTTAA), under which Federal agencies use technical standards developed 
or adopted by the VCSBs if compliance would not be inconsistent with 
applicable law or otherwise impracticable (see Section V.I of this 
preamble). The proposed copyrighted VCSB methods are available on their 
respective websites (standardmethods.org and astm.org) to everyone at a 
cost determined by the VCSB, generally from $60 to $80. Both 
organizations also offer memberships or subscriptions that allow 
unlimited access to their methods. The cost of obtaining these methods 
is not a significant financial burden for a discharger or environmental 
laboratory, making the methods reasonably available.
    This proposal also includes two vendor ATPs (see Section III.D of 
this preamble) and four revised EPA methods (see Section III.A of this 
preamble) which EPA proposes to incorporate by reference. The ATPs and 
EPA methods are available free of charge on their respective websites 
(sgsaxys.com/wp-content/uploads/2022/09/SGS-AXYS-Method-16130-Rev-1.0.pdf, pacelabs.com and epa.gov/cwa-methods/approved-cwa-chemical-test-methods), therefore the ATPs and EPA methods incorporated by 
reference are reasonably available.

V. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review Executive 
Order 13563: Improving Regulation and Regulatory Review

    This action is not a significant regulatory action and was 
therefore not submitted to the Office of Management and Budget (OMB) 
for review.

B. Paperwork Reduction Act

    This action does not impose an information collection burden under 
the Paperwork Reduction Act. This rule does not impose any information 
collection, reporting, or recordkeeping requirements. This proposal 
would merely add or revise CWA test procedures.

C. Regulatory Flexibility Act

    The Agency certifies that this action would not have a significant 
economic impact on a substantial number of small entities under the 
Regulatory Flexibility Act. This action would not impose any 
requirements on small entities. This action would approve new and 
revised versions of CWA testing procedures. Generally, these changes 
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. The proposed changes 
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., ASTM Method D7511). Because these methods would be alternatives 
rather than requirements, there are no direct costs associated with 
this 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 from the 
listed sources. See Section IV of this preamble.

D. Unfunded Mandates Reform Act

    This action does not contain any unfunded mandate as described in 
the Unfunded Mandates Reform Act, 2 U.S.C. 1531-1538, and does not 
significantly or uniquely affect small governments. The action imposes 
no enforceable duty on any state, local or tribal governments or the 
private sector.

E. Executive Order 13132: Federalism

    This proposed rule does not have federalism implications. It would 
not have substantial direct effects on the states, on the relationship 
between the national government and the states, or on the distribution 
of power and responsibilities among the various levels of government.

F. Executive Order 13175: Consultation and Coordination With Indian 
Tribal Governments

    This proposed rule does not have tribal implications as specified 
in Executive Order 13175. This rule would merely approve new and 
revised versions of test procedures. EPA does not expect the proposal 
would lead to any costs to any tribal governments, and if incurred, EPA 
projects they would be minimal. Thus, Executive Order 13175 does not 
apply to this action.

G. Executive Order 13045: Protection of Children From Environmental 
Health Risks and Safety Risks

    EPA interprets Executive Order 13045 as applying only to those 
regulatory actions that concern environmental health or safety risks 
that 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

[[Page 10741]]

significant regulatory action under Executive Order 12866.

I. National Technology Transfer and Advancement Act of 1995

    This action involves technical standards. 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 described above, this proposal is consistent with the 
NTTAA.

J. Executive Order 12898: Federal Actions To Address Environmental 
Justice in Minority Populations and Low-Income Populations

    Executive Order 12898 (59 FR 7629, February 16, 1994) directs 
Federal agencies, to the greatest extent practicable and permitted by 
law, to make environmental justice part of their mission by identifying 
and addressing, as appropriate, disproportionately high and adverse 
human health or environmental effects of their programs, policies, and 
activities on minority populations (people of color) and low-income 
populations.
    EPA believes that this type of action does not concern human health 
or environmental conditions and therefore cannot be evaluated with 
respect to potentially disproportionate and adverse effects on people 
of color, low-income populations and/or indigenous peoples. This action 
has no effect on human health or the environment because this action 
would approve new and revised versions of CWA testing procedures. The 
proposed changes 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. These proposed changes would provide 
increased flexibility for the regulated community in meeting monitoring 
requirements while improving data quality. In addition, this proposed 
update to the CWA methods would incorporate technological advances in 
analytical technology.

List of Subjects in 40 CFR Part 136

    Environmental protection, Incorporation by reference, Reporting and 
recordkeeping requirements, Test procedures, Water pollution control.

Michael S. Regan,
Administrator.
    For the reasons set out in the preamble, the EPA proposes to amend 
40 CFR part 136 as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS 
OF POLLUTANTS

0
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).
0
2. Amend Sec.  136.3 as follows:
0
a. Revise tables IA, IB, IC, ID, and IH in paragraph (a);
0
b. Revise the introductory text to paragraph (b) and paragraphs 
(b)(8)(ii) through (v), (b)(10)(i), (viii) through (xiv), (xvi) through 
(xxvi), (xxviii) through (xxxv), (xxxvii), (xxxix) through (li), (lv) 
through (lxiii), and (lxvii), (b)(15)(xi), (xx), (xxx), (xxxii), (lix), 
(lxv) through (lxvii), and (lxix);
0
c. Redesignate paragraphs (b)(33) through (39) as paragraphs (b)(35) 
through (41);
0
d. Add new paragraphs (b)(33) and (34); and
0
e. In paragraph (e), table II, revise Footnote ``5''.
    The revisions and additions read as follows:

Sec.  136.3  Identification of test procedures.

* * * * *

                                     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   Most Probable        p. 132; \3\ 1680;    9221 E-2014........
 gram dry weight.                  Number (MPN), 5      \11\ \15\ 1681
                                   tube, 3 dilution,    \11\ \20\.
                                   or
                                  Membrane filter      p. 124 \3\.........  9222 D-2015 \29\...
                                   (MF),\2\ \5\
                                   single step.
2. Coliform (fecal), number per   MPN, 5 tube, 3       p. 132 \3\.........  9221 E-2014; 9221 F-
 100 mL.                           dilution, or.                             2014 \33\.
                                  Multiple tube/       ...................  ...................  ........................  Colilert-18[supreg].\13\ \18\
                                   multiple well, or.                                                                       \28\
                                  MF,\2\ \5\ single    p. 124 \3\.........  9222 D-2015 \29\...  B-0050-85 \4\...........
                                   step \5\.
3. Coliform (total), number per   MPN, 5 tube, 3       p. 114 \3\.........  9221 B-2014........
 100 mL.                           dilution, or.
                                  MF,\2\ \5\ single    p. 108 \3\.........  9222 B-2015 \30\...  B-0025-85 \4\...........
                                   step or.
                                  MF,\2\ \5\ two step  p. 111 \3\.........  9222 B-2015 \30\...
                                   with enrichment.
4. E. coli, number per 100 mL...  MPN \6\ \8\ \16\     ...................  9221 B2014/9221 F-
                                   multiple tube, or.                        2014 \12\ \14\
                                                                             \33\.
                                  multiple tube/       ...................  9223 B-2016 \13\...  991.15 \10\.............  Colilert[supreg].\13\ \18\
                                   multiple well, or.                                                                      Colilert-18[supreg].\13\ \17\
                                                                                                                            \18\
                                  MF,\2\ \5\ \6\ \7\   ...................  9222 B-2015/9222 I-
                                   \8\ two step, or.                         2015 \31\.
                                  Single step........  1603.1 \21\........  ...................  ........................  m-ColiBlue24[supreg].\19\
5. Fecal streptococci, number     MPN, 5 tube, 3       p. 139 \3\.........  9230 B-2013........
 per 100 mL.                       dilution, or.
                                  MF,\2\ or..........  p. 136 \3\.........  9230 C-2013 \32\...  B-0055-85 \4\...........
                                  Plate count........  p. 143 \3\.........
6. Enterococci, number per 100    MPN, 5 tube, 3       p. 139 \3\.........  9230 B-2013........
 mL.                               dilution, or.

[[Page 10742]]

 
                                  MPN,\6\ \8\          ...................  9230 D-2013........  D6503-99 \9\............  Enterolert[supreg].\13\ \23\
                                   multiple tube/
                                   multiple well, or.
                                  MF \2\ \5\ \6\ \7\   1600.1 \24\........  9230 C-2013 \32\...
                                   \8\ single step or.
                                  Plate count........  p. 143 \3\.........
7. Salmonella, number per gram    MPN multiple tube..  1682 \22\..........
 dry weight \11\.
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                    Aquatic Toxicity
--------------------------------------------------------------------------------------------------------------------------------------------------------
8. Toxicity, acute, fresh water   Water flea,          2002.0 \25\........
 organisms, LC50, percent          Cladoceran,
 effluent.                         Ceriodaphnia dubia
                                   acute.
                                  Water fleas,         2021.0 \25\........
                                   Cladocerans,
                                   Daphnia pulex and
                                   Daphnia magna
                                   acute.
                                  Fish, Fathead        2000.0 \25\........
                                   minnow, Pimephales
                                   promelas, and
                                   Bannerfin shiner,
                                   Cyprinella leedsi,
                                   acute.
                                  Fish, Rainbow        2019.0 \25\........
                                   trout,
                                   Oncorhynchus
                                   mykiss, and brook
                                   trout, Salvelinus
                                   fontinalis, acute.
9. Toxicity, acute, estuarine     Mysid, Mysidopsis    2007.0 \25\.
 and marine organisms of the       bahia, acute.       ...................
 Atlantic Ocean and Gulf of       Fish, Sheepshead     2004.0 \25\........
 Mexico, LC50, percent effluent.   minnow, Cyprinodon
                                   variegatus, acute.
                                  Fish, Silverside,    2006.0 \25\........
                                   Menidia beryllina,
                                   Menidia menidia,
                                   and Menidia
                                   peninsulae, acute.
10. Toxicity, chronic, fresh      Fish, Fathead        1000.0 \26\........
 water organisms, NOEC or IC25,    minnow, Pimephales
 percent effluent.                 promelas, larval
                                   survival and
                                   growth.
                                  Fish, Fathead        1001.0 \26\........
                                   minnow, Pimephales
                                   promelas, embryo-
                                   larval survival
                                   and teratogenicity.
                                  Water flea,          1002.0 \26\........
                                   Cladoceran,
                                   Ceriodaphnia
                                   dubia, survival
                                   and reproduction.
                                  Green alga,          1003.0 \26\........
                                   Selenastrum
                                   capricornutum,
                                   growth.
11. Toxicity, chronic, estuarine  Fish, Sheepshead     1004.0 \27\........
 and marine organisms of the       minnow, Cyprinodon
 Atlantic Ocean and Gulf of        variegatus, larval
 Mexico, NOEC or IC25, percent     survival and
 effluent.                         growth.

[[Page 10743]]

 
                                  Fish, Sheepshead     1005.0 \27\........
                                   minnow, Cyprinodon
                                   variegatus, embryo-
                                   larval survival
                                   and teratogenicity.
                                  Fish, Inland         1006.0 \27\........
                                   silverside,
                                   Menidia beryllina,
                                   larval survival
                                   and growth.
                                  Mysid, Mysidopsis    1007.0 \27\........
                                   bahia, survival,
                                   growth, and
                                   fecundity.
                                  Sea urchin, Arbacia  1008.0 \27\........
                                   punctulata,
                                   fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[mu]m 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. U.S. 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.2-2014. 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.
\14\ After prior enrichment in a presumptive medium for total coliform using 9221B.2-2014, 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-2014. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [mu]g/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[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000 and the MPN calculated from the table provided by the manufacturer.
\17\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35[deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\18\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories, Inc.
\19\ A description of the mColiBlue24[supreg] 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\ Method 1603.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified
  mTEC), [in draft as of 2023]. U.S. EPA.
\22\ Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014.
  U.S. EPA.
\23\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\24\ Method 1600.1: Enterococci in Water by Membrane Filtration Using Membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), [in draft as of
  2023]. U.S. EPA.
\25\ 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; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\26\ 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; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\27\ 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; and U.S. EPA Whole Effluent Toxicity Methods Errata Sheet, EPA 821-R-02-012-ES. December 2016.
\28\ To use Colilert-18[supreg] to assay for fecal coliforms, the incubation temperature is 44.5  0.2 [deg]C, and a water bath incubator is
  used.
\29\ On a monthly basis, at least ten blue colonies from positive samples must be verified using Lauryl Tryptose Broth and EC broth, followed by count
  adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications
  should be done from randomized sample sources.
\30\ On a monthly basis, at least ten sheen colonies from positive samples must be verified using lauryl tryptose broth and brilliant green lactose bile
  broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using lauryl tryptose broth.
  Where possible, verifications should be done from randomized sample sources.

[[Page 10744]]

 
\31\ Subject coliform positive samples determined by 9222 B-2015 or other membrane filter procedure to 9222 I-2015 using NA-MUG media.
\32\ Verification of colonies by incubation of BHI agar at 10  0.5 [deg]C for 48  3 h is optional. As per the Errata to the 23rd
  Edition of Standard Methods for the Examination of Water and Wastewater ``Growth on a BHI agar plate incubated at 10  0.5 [deg]C for 48
   3 h is further verification that the colony belongs to the genus Enterococcus.''
\33\ 9221F. 2-2014 allows for simultaneous detection of E. coli and thermotolerant fecal coliforms by adding inverted vials to EC-MUG; the inverted
  vials collect gas produced by thermotolerant fecal coliforms.

                                                  Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                  Methodology \58\            EPA \52\         Standard methods \84\           ASTM             USGS/AOAC/other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L.........  Electrometric endpoint  ......................  2310 B-2020..........  D1067-16.............  I-1020-85.\2\
                                      or phenolphthalein
                                      endpoint.
2. Alkalinity, as CaCO3, mg/L......  Electrometric or        ......................  2320 B-2021..........  D1067-16.............  973.43,\3\ I-1030-
                                      Colorimetric                                                                                  85.\2\
                                      titration to pH 4.5,
                                      Manual.
                                     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    ......................  3111 D-2019 or 3111 E- .....................  I-3051-85.\2\
                                      \36\.                                           2019.
                                     AA furnace............  ......................  3113 B-2020..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2          3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003),\68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     Direct Current Plasma   ......................  .....................  D4190-15.............  See footnote.\34\
                                      (DCP) \36\.
                                     Colorimetric            ......................  3500-Al B-2020.......
                                      (Eriochrome cyanine
                                      R).
4. Ammonia (as N), mg/L............  Manual distillation     350.1, Rev. 2.0 (1993)  4500-NH3 B-2021......  .....................  973.49.\3\
                                      \6\ or gas diffusion
                                      (pH > 11), followed
                                      by any of the
                                      following:
                                     Nesslerization........  ......................  .....................  D1426-15 (A).........  973.49,\3\ I-3520-
                                                                                                                                    85.\2\
                                     Titration.............  ......................  4500-NH3 C-2021......
                                     Electrode.............  ......................  4500-NH3 D-2021 or E-  D1426-15 (B).........
                                                                                      2021.
                                     Manual phenate,         ......................  4500-NH3 F-2021......  .....................  See footnote.\60\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction-
                                      based methods.
                                     Automated phenate,      350.1,\30\ Rev. 2.0     4500-NH3 G-2021 4500-  .....................  I-4523-85,\2\ I-2522-
                                      salicylate, or other    (1993).                 NH3 H-2021.                                   90.\80\
                                      substituted phenols
                                      in Berthelot reaction-
                                      based methods.
                                     Automated electrode...  ......................  .....................  .....................  See footnote.\7\
                                     Ion Chromatography....  ......................  .....................  D6919-17.............
                                     Automated gas           ......................  .....................  .....................  Timberline Ammonia-
                                      diffusion, followed                                                                           001.\74\
                                      by conductivity cell
                                      analysis.
                                     Automated gas           ......................  .....................  .....................  FIAlab100.\82\
                                      diffusion followed by
                                      fluorescence detector
                                      analysis.
5. Antimony--Total, \4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019..........
                                      \36\.
                                     AA furnace............  ......................  3113 B-2020..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).

[[Page 10745]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
6. Arsenic--Total,\4\ mg/L.........  Digestion,\4\ followed  206.5 (Issued 1978)
                                      by any of the           \1\.
                                      following:
                                     AA gaseous hydride....  ......................  3114 B-2020 or 3114 C- D2972-15 (B).........  I-3062-85.\2\
                                                                                      2020.
                                     AA furnace............  ......................  3113 B-2020..........  D2972-15 (C).........  I-4063-98.\49\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     Colorimetric (SDDC)...  ......................  3500-As B-2020.......  D2972-15 (A).........  I-3060-85.\2\
7. Barium--Total,\4\ mg/L..........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 D-2019..........  .....................  I-3084-85.\2\
                                      \36\.
                                     AA furnace............  ......................  3113 B-2020..........  D4382-18.............
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  .....................  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  .....................  See footnote.\34\
8. Beryllium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2019 or 3111 E- D3645-15 (A).........  I-3095-85.\2\
                                                                                      2019.
                                     AA furnace............  ......................  3113 B-2020..........  D3645-15 (B).........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP...................  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric            ......................  See footnote.\61\....
                                      (aluminon).
9. Biochemical oxygen demand         Dissolved Oxygen        ......................  5210 B-2016 \85\.....  .....................  973.44,\3\ p. 17,\9\
 (BOD5), mg/L.                        Depletion.                                                                                    I-1578-78,\8\ See
                                                                                                                                    footnote.\10\ \63\
10. Boron--Total,\37\ mg/L.........  Colorimetric            ......................  4500-B B-2011........  .....................  I-3112-85.\2\
                                      (curcumin).
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  D4190-15.............  See footnote.\34\
11. Bromide, mg/L..................  Electrode.............  ......................  .....................  D1246-16.............  I-1125-85.\2\
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2020, C-2020    D4327-17.............  993.30,\3\ I-2057-
                                                              and 300.1, Rev 1.0      or D-2020.                                    85.\79\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
12. Cadmium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D3557-17 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2019.                                         I-3135-85 \2\ or I-
                                                                                                                                    3136-85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D3557-17 (D).........  I-4138-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............  I-1472-85 \2\ or I-
                                                              \68\ 200.7, Rev. 4.4                                                  4471-97.\50\
                                                              (1994).

[[Page 10746]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Voltammetry \11\......  ......................  .....................  D3557-17 (C).........
                                     Colorimetric            ......................  3500-Cd-D-1990.......
                                      (Dithizone).
13. Calcium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019 or 3111 D- D511-14 (B)..........  I-3152-85.\2\
                                                                                      2019.
                                     ICP/AES...............  200.5, Rev 4.2 (2003);  3120 B-2020..........  .....................  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Titrimetric (EDTA)....  ......................  3500-Ca B-2020.......  D511-14 (A)..........
                                     Ion Chromatography....  ......................  .....................  D6919-17.............
14. Carbonaceous biochemical oxygen  Dissolved Oxygen        ......................  5210 B-2016 \85\.....  .....................  See footnote.\35\
 demand (CBOD5), mg/L \12\.           Depletion with                                                                                \63\
                                      nitrification
                                      inhibitor.
15. Chemical oxygen demand (COD),    Titrimetric...........  410.3 (Rev. 1978) \1\.  5220 B-2011 or C-2011  D1252-06(12) (A).....  973.46,\3\ p. 17,\9\
 mg/L.                                                                                                                              I-3560-85.\2\
                                     Spectrophotometric,     410.4, Rev. 2.0 (1993)  5220 D-2011..........  D1252-06(12) (B).....  See footnotes,\13\
                                      manual or automatic.                                                                          \14\ \83\ I-3561-
                                                                                                                                    85.\2\
16. Chloride, mg/L.................  Titrimetric: (silver    ......................  4500-Cl- B-2021......  D512-12 (B)..........  I-1183-85.\2\
                                      nitrate).
                                     (Mercuric nitrate)....  ......................  4500-Cl- C-2021......  D512-12 (A)..........  973.51,\3\ I-1184-
                                                                                                                                    85.\2\
                                     Colorimetric: manual..  ......................  .....................  .....................  I-1187-85.\2\
                                     Automated               ......................  4500-Cl- E-2021......  .....................  I-2187-85.\2\
                                      (ferricyanide).
                                     Potentiometric          ......................  4500-Cl- D-2021......
                                      Titration.
                                     Ion Selective           ......................  .....................  D512-12 (C)..........
                                      Electrode.
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2020 or 4110 C- D4327-17.............  993.30,\3\ I-2057-
                                                              and 300.1, Rev 1.0      2020.                                         90.\51\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
17. Chlorine--Total residual, mg/L.  Amperometric direct...  ......................  4500-Cl D-2011.......  D1253-14.............
                                     Amperometric direct     ......................  4500-Cl E-2011.......
                                      (low level).
                                     Iodometric direct.....  ......................  4500-Cl B-2011.......
                                     Back titration ether    ......................  4500-Cl C-2011.......
                                      end-point \15\.
                                     DPD-FAS...............  ......................  4500 Cl F-2011.......
                                     Spectrophotometric,     ......................  4500-Cl G-2011.......
                                      DPD.
                                     Electrode.............  ......................  .....................  .....................  See footnote.\16\
17A. Chlorine-Free Available, mg/L.  Amperometric direct...  ......................  4500-Cl D-2011.......  D1253-14.............
                                     Amperometric direct     ......................  4500-Cl E-2011.......
                                      (low level).
                                     DPD-FAS...............  ......................  4500-Cl F-2011.......
                                     Spectrophotometric,     ......................  4500-Cl G-2011.......
                                      DPD.
18. Chromium VI dissolved, mg/L....  0.45-micron filtration
                                      followed by any of
                                      the following:
                                     AA chelation-           ......................  3111 C-2019..........  .....................  I-1232-85.\2\
                                      extraction.
                                     Ion Chromatography....  218.6, Rev. 3.3 (1994)  3500-Cr C-2020.......  D5257-17.............  993.23.\3\
                                     Colorimetric (diphenyl- ......................  3500-Cr B-2020.......  D1687-17 (A).........  I-1230-85.\2\
                                      carbazide).

[[Page 10747]]

 
19. Chromium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019..........  D1687-17 (B).........  974.27,\3\ I-3236-
                                      \36\.                                                                                         85.\2\
                                     AA chelation-           ......................  3111 C-2019..........
                                      extraction.
                                     AA furnace............  ......................  3113 B-2020..........  D1687-17 (C).........  I-3233-93.\46\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2          3120 B-2020..........  D1976-20.............
                                                              (2003),\68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-05
                                                                                                                                    \70\ I-4472-97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric (diphenyl- ......................  3500-Cr B-2020.......
                                      carbazide).
20. Cobalt--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019 or 3111 C- D3558-15 (A or B)....  p. 37,\9\ I-3239-
                                                                                      2019.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D3558-15 (C).........  I-4243-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-05
                                                                                                                                    \70\ I-4472-97.\81\
                                     DCP...................  ......................  .....................  D4190-15.............  See footnote.\34\
21. Color, platinum cobalt units or  Colorimetric (ADMI)...  ......................  2120 F-2021 \78\.....
 dominant wavelength, hue,
 luminance purity.
                                     Platinum cobalt visual  ......................  2120 B-2021..........  .....................  I-1250-85.\2\
                                      comparison.
                                     Spectrophotometric....  ......................  .....................  .....................  See footnote.\18\
22. Copper--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D1688-17 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2019.                                         I-3270-85 \2\ or I-
                                                                                                                                    3271-85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D1688-17 (C).........  I-4274-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05,\70\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Cu B-2020.......
                                      (Neocuproine).
                                     Colorimetric            ......................  3500-Cu C-2020.......  .....................  See footnote.\19\
                                      (Bathocuproine).
23. Cyanide--Total, mg/L...........  Automated UV digestion/ ......................  .....................  .....................  Kelada-01.\55\
                                      distillation and
                                      Colorimetry.
                                     Segmented Flow          ......................  4500-CN- P-2021......  D7511-12(17).........
                                      Injection, In-Line
                                      Ultraviolet
                                      Digestion, followed
                                      by gas diffusion
                                      amperometry.
                                     Manual distillation     335.4, Rev. 1.0 (1993)  4500-CN- B-2021 and C- D2036-09(15)(A),       10-204-00-1-X.\56\
                                      with MgCl2, followed    \57\.                   2021.                  D7284-20.
                                      by any of the
                                      following:
                                     Flow Injection, gas     ......................  .....................  D2036-09(15)(A) D7284-
                                      diffusion amperometry.                                                 20.

[[Page 10748]]

 
                                     Titrimetric...........  ......................  4500-CN- D-2021......  D2036-09(15)(A)......  p. 22.\9\
                                     Spectrophotometric,     ......................  4500-CN- E-2021......  D2036-09(15)(A)......  I-3300-85.\2\
                                      manual.
                                     Semi-Automated \20\...  335.4, Rev. 1.0 (1993)  4500-CN- N-2021......  .....................  10-204-00-1-X,\56\ I-
                                                              \57\.                                                                 4302-85.\2\
                                     Ion Chromatography....  ......................  .....................  D2036-09(15)(A)......
                                     Ion Selective           ......................  4500-CN- F-2021......  D2036-09(15)(A)......
                                      Electrode.
24. Cyanide-Available, mg/L........  Cyanide Amenable to     ......................  4500-CN- G-2021......  D2036-09(15)(B)......
                                      Chlorination (CATC);
                                      Manual distillation
                                      with MgCl2, followed
                                      by Titrimetric or
                                      Spectrophotometric.
                                     Flow injection and      ......................  4500-CN- Q-2021......  D6888-16.............  OIA-1677-09.\44\
                                      ligand exchange,
                                      followed by gas
                                      diffusion amperometry
                                      \59\.
                                     Automated Distillation  ......................  .....................  .....................  Kelada-01.\55\
                                      and Colorimetry (no
                                      UV digestion).
24. A Cyanide-Free, mg/L...........  Flow Injection,         ......................  4500-CN- R-2021......  D7237-18 (A).........  OIA-1677-09.\44\
                                      followed by gas
                                      diffusion amperometry.
                                     Manual micro-diffusion  ......................  .....................  D4282-15.............
                                      and colorimetry.
25. Fluoride--Total, mg/L..........  Manual                  ......................  4500-F- B-2021.......  D1179-16 (A).........
                                      distillation,\6\
                                      followed by any of
                                      the following:
                                     Electrode, manual.....  ......................  4500-F- C-2021.......  D1179-16 (B).........
                                     Electrode, automated..  ......................  4500-F- G-2021.......  .....................  I-4327-85.\2\
                                     Colorimetric, (SPADNS)  ......................  4500-F- D-2021.......
                                     Automated complexone..  ......................  4500-F- E-2021.......
                                     Ion Chromatography....  300.0, Rev 2.1 (1993)   4110 B-2020 or C-2020  D4327-17.............  993.30.\3\
                                                              and 300.1, Rev 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
26. Gold--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........
                                     AA furnace............  231.2 (Issued 1978)     3113 B-2020..........
                                                              \1\.
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
27. Hardness--Total, as CaCO3, mg/L  Automated colorimetric  130.1 (Issued 1971)
                                                              \1\.
                                     Titrimetric (EDTA)....  ......................  2340 C-2021..........  D1126-17.............  973.52B,\3\ I-1338-
                                                                                                                                    85.\2\
                                     Ca plus Mg as their     ......................  2340 B-2021..........
                                      carbonates, by any
                                      approved method for
                                      Ca and Mg (See
                                      Parameters 13 and
                                      33), provided that
                                      the sum of the lowest
                                      point of quantitation
                                      for Ca and Mg is
                                      below the NPDES
                                      permit requirement
                                      for Hardness.
28. Hydrogen ion (pH), pH units....  Electrometric           ......................  4500-H\+\ B-2021.....  D1293-18 (A or B)....  973.41,\3\ I-1586-
                                      measurement.                                                                                  85.\2\
                                     Automated electrode...  150.2 (Dec. 1982) \1\.  .....................  .....................  See footnote,\21\ I-
                                                                                                                                    2587-85.\2\

[[Page 10749]]

 
29. Iridium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........
                                     AA furnace............  235.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2020..........
30. Iron--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D1068-15 (A).........  974.27,\3\ I-3381-
                                      \36\.                                           2019.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D1068-15 (B).........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Fe B-2011.......  D1068-15 (C).........  See footnote.\22\
                                      (Phenanthroline).
31. Kjeldahl Nitrogen \5\--Total,    Manual digestion \20\   ......................  4500-Norg B-2021 or C- D3590-17 (A).........  I-4515-91.\45\
 (as N), mg/L.                        and distillation or                             2021 and 4500-NH3 B-
                                      gas diffusion,                                  2021.
                                      followed by any of
                                      the following:
                                     Titration.............  ......................  4500-NH3 C-2021......  .....................  973.48.\3\
                                     Nesslerization........  ......................  .....................  D1426-15 (A).........
                                     Electrode.............  ......................  4500-NH3 D-2021 or E-  D1426-15 (B).........
                                                                                      2021.
                                     Semi-automated phenate  350.1, Rev. 2.0 (1993)  4500-NH3 G-2021 or
                                                                                      4500-NH3 H-2021.
                                     Manual phenate,         ......................  4500-NH3 F-2021......  .....................  See footnote.\60\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction
                                      based methods.
                                     Automated gas           ......................  .....................  .....................  Timberline Ammonia-
                                      diffusion, followed                                                                           001.\74\
                                      by conductivity cell
                                      analysis.
                                     Automated gas           ......................  .....................  .....................  FIAlab 100.\82\
                                      diffusion followed by
                                      fluorescence detector
                                      analysis.
                                                              Automated Methods for TKN that do not require manual distillation
                                     Automated phenate,      351.1 (Rev. 1978) \1\.  .....................  .....................  I-4551-78.\8\
                                      salicylate, or other
                                      substituted phenols
                                      in Berthelot reaction-
                                      based methods
                                      colorimetric (auto
                                      digestion and
                                      distillation).
                                     Semi-automated block    351.2, Rev. 2.0 (1993)  4500-Norg D-2021.....  D3590-17 (B).........  I-4515-91.\45\
                                      digestor colorimetric
                                      (distillation not
                                      required).
                                     Block digester,         ......................  .....................  .....................  See footnote.\39\
                                      followed by Auto
                                      distillation and
                                      Titration.
                                     Block digester,         ......................  .....................  .....................  See footnote.\40\
                                      followed by Auto
                                      distillation and
                                      Nesslerization.
                                     Block Digester,         ......................  .....................  .....................  See footnote.\41\
                                      followed by Flow
                                      injection gas
                                      diffusion
                                      (distillation not
                                      required).

[[Page 10750]]

 
                                     Digestion with          ......................  .....................  .....................  Hach 10242.\76\
                                      peroxdisulfate,
                                      followed by
                                      Spectrophotometric
                                      (2,6-dimethyl phenol).
                                     Digestion with          ......................  .....................  .....................  NCASI TNTP
                                      persulfate, followed                                                                          W10900.\77\
                                      by Colorimetric.
32. Lead--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D3559-15 (A or B)....  974.27,\3\ I-3399-
                                      \36\.                                           2019.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D3559-15 (D).........  I-4403-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Voltammetry \11\......  ......................  .....................  D3559-15 (C).........
                                     Colorimetric            ......................  3500-Pb B-2020.......
                                      (Dithizone).
33. Magnesium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........  D511-14 (B)..........  974.27,\3\ I-3447-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Ion Chromatography....  ......................  .....................  D6919-17.............
34. Manganese--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D858-17 (A or B).....  974.27,\3\ I-3454-
                                      \36\.                                           2019.                                         85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  D858-17 (C)..........
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric            ......................  3500-Mn B-2020.......  .....................  920.203.\3\
                                      (Persulfate).
                                     Colorimetric            ......................  .....................  .....................  See footnote.\23\
                                      (Periodate).
35. Mercury--Total, mg/L...........  Cold vapor, Manual....  245.1, Rev. 3.0 (1994)  3112 B-2020..........  D3223-17.............  977.22,\3\ I-3462-
                                                                                                                                    85.\2\
                                     Cold vapor, Automated.  245.2 (Issued 1974)
                                                              \1\.
                                     Cold vapor atomic       245.7 Rev. 2.0 (2005)   .....................  .....................  I-4464-01.\71\
                                      fluorescence            \17\.
                                      spectrometry (CVAFS).
                                     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-2019..........  .....................  I-3490-85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  .....................  I-3492-96.\47\
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2020..........  D1976-20.............  I-4471-97.\50\

[[Page 10751]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
37. Nickel--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D1886-14 (A or B)....  I-3499-85.\2\
                                      \36\.                                           2019.
                                     AA furnace............  ......................  3113 B-2020..........  D1886-14 (C).........  I-4503-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05,\70\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
38. Nitrate (as N), mg/L...........  Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2020 or C-2020  D4327-17.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
                                     Ion Selective           ......................  4500-NO3- D-2019.....
                                      Electrode.
                                     Colorimetric (Brucine   352.1 (Issued 1971)     .....................  .....................  973.50,\3\ 419D,\86\
                                      sulfate).               \1\.                                                                  p. 28.\9\
                                     Spectrophotometric      ......................  .....................  .....................  Hach 10206.\75\
                                      (2,6-dimethylphenol).
                                     Nitrate-nitrite N
                                      minus Nitrite N (See
                                      parameters 39 and 40).
39. Nitrate-nitrite (as N), mg/L...  Cadmium reduction,      ......................  4500-NO3- E-2019.....  D3867-16 (B).........
                                      Manual.
                                     Cadmium reduction,      353.2, Rev. 2.0 (1993)  4500-NO3- F-2019 or    D3867-16 (A).........  I-2545-90.\51\
                                      Automated.                                      4500-NO3- I-2019.
                                     Automated hydrazine...  ......................  4500-NO3- H-2019.....
                                     Reduction/Colorimetric  ......................  .....................  .....................  See footnote.\62\
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2020 or C-2020  D4327-17.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
                                     Enzymatic reduction,    ......................  .....................  D7781-14.............  I-2547-11,\72\ I-2548-
                                      followed by automated                                                                         11,\72\ N07-
                                      colorimetric                                                                                  0003.\73\
                                      determination.
                                     Enzymatic reduction,    ......................  4500-NO3- J-2018.....
                                      followed by manual
                                      colorimetric
                                      determination.
                                     Spectrophotometric      ......................  .....................  .....................  Hach 10206.\75\
                                      (2,6-dimethylphenol).
40. Nitrite (as N), mg/L...........  Spectrophotometric:     ......................  4500-NO2- B-2021.....  .....................  See footnote.\25\
                                      Manual.
                                     Automated               ......................  .....................  .....................  I-4540-85,\2\ See
                                      (Diazotization).                                                                              footnote.\62\ I-2540-
                                                                                                                                    90.\80\
                                     Automated (*bypass      353.2, Rev. 2.0 (1993)  4500-NO3- F-2019 4500- D3867-16 (A).........  I-4545-85.\2\
                                      cadmium reduction).                             NO3- I-2019.
                                     Manual (*bypass         ......................  4500-NO3- E-2019,      D3867-16 (B).........
                                      cadmium or enzymatic                            4500-NO3- J-2018.
                                      reduction).
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2020 or C-2020  D4327-17.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
                                     Automated (*bypass      ......................  .....................  D7781-14.............  I-2547-11,\72\ I-2548-
                                      Enzymatic reduction).                                                                         11,\72\ N07-
                                                                                                                                    0003.\73\

[[Page 10752]]

 
41. Oil and grease--Total            Hexane extractable      1664 Rev. A; 1664 Rev.  5520 B or G-2021 \38\
 recoverable, mg/L.                   material (HEM): n-      B \42\.
                                      Hexane extraction and
                                      gravimetry.
                                     Silica gel treated HEM  1664 Rev. A; 1664 Rev.  5520 B or G-2021 \38\
                                      (SGT-HEM): Silica gel   B \42\.                 and 5520 F-2021 \38\.
                                      treatment and
                                      gravimetry.
42. Organic carbon--Total (TOC), mg/ Combustion............  ......................  5310 B-2014..........  D7573-18a \e1\.......  973.47,\3\ p. 14 \24\
 L.
                                     Heated persulfate or    ......................  5310 C-2014 5310 D-    D4839-03(17).........  973.47,\3\ p. 14.\24\
                                      UV persulfate                                   2011.
                                      oxidation.
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-2021 or G-    .....................  973.56,\3\ I-4601-
                                                                                      2021.                                         85,\2\ I-2601-
                                                                                                                                    90.\80\
                                     Manual, single-reagent  ......................  4500-P E-2021........  D515-88 (A)..........  973.55.\3\
                                     Manual, two-reagent...  365.3 (Issued 1978)
                                                              \1\.
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2020 or C-2020  D4327-17.............  993.30.\3\
                                                              and 300.1, Rev. 1.0
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
45. Osmium--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2019..........
                                     AA furnace............  252.2 (Issued 1978)
                                                              \1\.
46. Oxygen, dissolved, mg/L........  Winkler (Azide          ......................  4500-O (B-F)-2021....  D888-18 (A)..........  973.45B,\3\ I-1575-
                                      modification).                                                                                78.\8\
                                     Electrode.............  ......................  4500-O G-2021........  D888-18 (B)..........  I-1576-78.\8\
                                     Luminescence-Based      ......................  4500-O H-2021........  D888-18 (C)..........  See footnote.\63\ See
                                      Sensor.                                                                                       footnote.\64\
47. Palladium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........
                                     AA furnace............  253.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2020..........
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
48. Phenols, mg/L..................  Manual                  420.1 (Rev. 1978) \1\.  5530 B-2021..........  D1783-01(12).........
                                      distillation,\26\
                                      followed by any of
                                      the following:.
                                     Colorimetric (4AAP)     420.1 (Rev. 1978) \1\.  5530 D-2021 \27\.....  D1783-01(12) (A or B)
                                      manual.
                                     Automated colorimetric  420.4 Rev. 1.0 (1993).
                                      (4AAP).
49. Phosphorus (elemental), mg/L...  Gas-liquid              ......................  .....................  .....................  See footnote.\28\
                                      chromatography.
50. Phosphorus--Total, mg/L........  Digestion,\20\          ......................  4500-P B (5)-2021....  .....................  973.55.\3\
                                      followed by any of
                                      the following:
                                     Manual................  365.3 (Issued 1978)     4500-P E-2021........  D515-88 (A)..........
                                                              \1\.
                                     Automated ascorbic      365.1 Rev. 2.0 (1993).  4500-P (F-H)-2021....  .....................  973.56,\3\ I-4600-
                                      acid reduction.                                                                               85.\2\
                                     ICP/AES \4\ \36\......  200.7, Rev. 4.4 (1994)  3120 B-2020..........  .....................  I-4471-97.\50\
                                     Semi-automated block    365.4 (Issued 1974)     .....................  D515-88 (B)..........  I-4610-91.\48\
                                      digestor (TKP           \1\.
                                      digestion).
                                     Digestion with          ......................  .....................  .....................  NCASI TNTP
                                      persulfate, followed                                                                          W10900.\77\
                                      by Colorimetric.
51. Platinum--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........

[[Page 10753]]

 
                                     AA furnace............  255.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2020..........
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
52. Potassium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........  .....................  973.53,\3\ I-3630-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2020..........
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     Flame photometric.....  ......................  3500-K B-2020........
                                     Electrode.............  ......................  3500-K C-2020........
                                     Ion Chromatography....  ......................  .....................  D6919-17.............
53. Residue--Total, mg/L...........  Gravimetric, 103-       ......................  2540 B-2020..........  .....................  I-3750-85.\2\
                                      105[deg].
54. Residue--filterable, mg/L......  Gravimetric, 180[deg].  ......................  2540 C-2020..........  D5907-18 (B).........  I-1750-85.\2\
55. Residue--non-filterable (TSS),   Gravimetric, 103-       ......................  2540 D-2020..........  D5907-18 (A).........  I-3765-85.\2\
 mg/L.                                105[deg] post-washing
                                      of residue.
56. Residue--settleable, mg/L......  Volumetric (Imhoff      ......................  2540 F-2020..........
                                      cone), or gravimetric.
57. Residue--Volatile, mg/L........  Gravimetric, 550[deg].  160.4 (Issued 1971)     2540 E-2020..........  .....................  I-3753-85.\2\
                                                              \1\.
58. Rhodium--Total,\4\ mg/L........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration,   ......................  3111 B-2019..........
                                      or.
                                     AA furnace............  265.2 (Issued 1978)
                                                              \1\.
                                     ICP/MS................  ......................  3125 B-2020..........
59. Ruthenium--Total,\4\ mg/L......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration,   ......................  3111 B-2019..........
                                      or.
                                     AA furnace............  267.2 \1\.............
                                     ICP/MS................  ......................  3125 B-2020..........
60. Selenium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA furnace............  ......................  3113 B-2020..........  D3859-15 (B).........  I-4668-98.\49\
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES \36\..........  200.5, Rev 4.2 (2003);  3120 B-2020..........  D1976-20.............
                                                              \68\ 200.7, Rev. 4.4
                                                              (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05,\70\ I-4472-
                                                                                                                                    97.\81\
                                     AA gaseous hydride....  ......................  3114 B-2020, or 3114   D3859-15 (A).........  I-3667-85.\2\
                                                                                      C-2020.
61. Silica--Dissolved,\37\ mg/L....  0.45-micron filtration
                                      followed by any of
                                      the following:
                                     Colorimetric, Manual..  ......................  4500-SiO2 C-2021.....  D859-16..............  I-1700-85.\2\
                                     Automated               ......................  4500-SiO2 E-2021 or F- .....................  I-2700-85.\2\
                                      (Molybdosilicate).                              2021.
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2020..........  .....................  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
62. Silver--Total,\4\ \31\ mg/L....  Digestion,\4\ \29\
                                      followed by any of
                                      the following:
                                     AA direct aspiration..  ......................  3111 B-2019 or 3111 C- .....................  974.27,\3\ p. 37,\9\
                                                                                      2019.                                         I-3720-85.\2\
                                     AA furnace............  ......................  3113 B-2020..........  .....................  I-4724-89.\51\
                                     STGFAA................  200.9, Rev. 2.2 (1994)

[[Page 10754]]

 
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4472-
                                                                                                                                    97.\81\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
63. Sodium--Total,\4\ mg/L.........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........  .....................  973.54,\3\ I-3735-
                                                                                                                                    85.\2\
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2020..........  .....................  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
                                     Flame photometric.....  ......................  3500-Na B-2020.......
                                     Ion Chromatography....  ......................  .....................  D6919-17.............
64. Specific conductance, micromhos/ Wheatstone bridge.....  120.1 (Rev. 1982) \1\.  2510 B-2021..........  D1125-95(99) (A).....  973.40,\3\ I-2781-
 cm at 25 [deg]C.                                                                                                                   85.\2\
65. Sulfate (as SO4), mg/L.........  Automated colorimetric  375.2, Rev. 2.0 (1993)  4500-SO42- F-2021 or
                                                                                      G-2021.
                                     Gravimetric...........  ......................  4500-SO42- C-2021 or   .....................  925.54. \3\
                                                                                      D-2021.
                                     Turbidimetric.........  ......................  4500-SO42- E-2021....  D516-16..............
                                     Ion Chromatography....  300.0, Rev. 2.1 (1993)  4110 B-2020 or C-2020  D4327-17.............  993.30,\3\ I-4020-
                                                              and 300.1, Rev. 1.0                                                   05.\70\
                                                              (1997).
                                     CIE/UV................  ......................  4140 B-2020..........  D6508-15.............  D6508, Rev. 2.\54\
66. Sulfide (as S), mg/L...........  Sample Pretreatment...  ......................  4500-S2- B, C-2021...
                                     Titrimetric (iodine)..  ......................  4500-S2- F-2021......  .....................  I-3840-85.\2\
                                     Colorimetric            ......................  4500-S2- D-2021......
                                      (methylene blue).
                                     Ion Selective           ......................  4500-S2- G-2021......  D4658-15.............
                                      Electrode.
67. Sulfite (as SO3), mg/L.........  Titrimetric (iodine-    ......................  4500-SO32- B-2021....
                                      iodate).
68. Surfactants, mg/L..............  Colorimetric            ......................  5540 C-2021..........  D2330-20.............
                                      (methylene blue).
69. Temperature, [deg]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-2019..........
                                     AA furnace............  279.2 (Issued 1978)     3113 B-2020..........
                                                              \1\.
                                     STGFAA................  200.9, Rev. 2.2 (1994)
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)  3120 B-2020..........  D1976-20.............
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4471-
                                                                                                                                    97,\50\ I-4472-
                                                                                                                                    97.\81\
71. Tin--Total,\4\ mg/L............  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 B-2019..........  .....................  I-3850-78.\8\
                                     AA furnace............  ......................  3113 B-2020..........
                                     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-2020..........  D5673-16.............  993.14.\3\
72. Titanium--Total,\4\ mg/L.......  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration..  ......................  3111 D-2019..........
                                     AA furnace............  283.2 (Issued 1978)
                                                              \1\.
                                     ICP/AES...............  200.7, Rev. 4.4 (1994)

[[Page 10755]]

 
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14.\3\
                                     DCP...................  ......................  .....................  .....................  See footnote.\34\
73. Turbidity, NTU \53\............  Nephelometric.........  180.1, Rev. 2.0 (1993)  2130 B-2020..........  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-2019..........
                                     AA furnace............  ......................  3113 B-2020..........  D3373-17.............
                                     ICP/AES...............  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05.\70\
                                     DCP...................  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric (Gallic    ......................  3500-V B-2011........
                                      Acid).
75. Zinc--Total,\4\ mg/L...........  Digestion,\4\ followed
                                      by any of the
                                      following:
                                     AA direct aspiration    ......................  3111 B-2019 or 3111 C- D1691-17 (A or B)....  974.27,\3\ p. 37,\9\
                                      \36\.                                           2019.                                         I-3900-85.\2\
                                     AA furnace............  289.2 (Issued 1978)
                                                              \1\.
                                     ICP/AES \36\..........  200.5, Rev. 4.2         3120 B-2020..........  D1976-20.............  I-4471-97.\50\
                                                              (2003); \68\ 200.7,
                                                              Rev. 4.4 (1994).
                                     ICP/MS................  200.8, Rev. 5.4 (1994)  3125 B-2020..........  D5673-16.............  993.14,\3\ I-4020-
                                                                                                                                    05,\70\ I-4472-
                                                                                                                                    97.\81\
                                     DCP \36\..............  ......................  .....................  D4190-15.............  See footnote.\34\
                                     Colorimetric (Zincon).  ......................  3500 Zn B-2020.......  .....................  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 Chemical Analysis of Water and Wastes) is required prior to analysis. The procedure used should subject the sample to
  gentle acid refluxing, and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption (FLAA) determinations, a
  combination acid (nitric and hydrochloric acids) digestion is preferred, prior 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
  of this section); the total recoverable digestion procedures in EPA Methods 200.7, 200.8, and 200.9 may be used for those respective methods.
  Regardless of the digestion procedure, the results of the analysis after digestion procedure are reported as ``total'' metals.
\5\ Copper sulfate or other catalysts that have been found suitable may be used in place of mercuric sulfate.
\6\ Manual distillation is not required if comparability data on representative 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 (for 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.

[[Page 10756]]

 
\12\ Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test method which measures ``total 5-day BOD.'' The
  addition of the nitrification inhibitor is not a procedural option but must be included to report the CBOD5 parameter. A discharger whose permit
  requires reporting the traditional BOD5 may not use a nitrification inhibitor in the procedure for reporting the results. Only when a discharger's
  permit specifically states CBOD5 is required can the permittee report data using a nitrification inhibitor.
\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 253 (1971) and Technical Bulletin 803, May 2000.
\19\ Method 8506, Bicinchoninate 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 Chromatography,
  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 Na2S2O3 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 NH4OH, 6.5 g of KCN, and 5.0 mL of a 1.0 N solution of I2
  to 50 mL of reagent water in a volumetric flask and dilute to 100.0 mL. After digestion of the sample, adjust the pH of the digestate to >7 to prevent
  the formation of HCN under acidic conditions. Add 1 mL of the cyanogen iodide solution to the sample digestate and adjust the volume to 100 mL with
  reagent water (NOT acid). If cyanogen iodide is added to sample digestates, then silver standards must be prepared that contain cyanogen iodide as
  well. Prepare working standards by diluting a small volume of a silver stock solution with water and adjusting the pH >7 with NH4OH. Add 1 mL of the
  cyanogen iodide solution and let stand 1 hour. Transfer to a 100-mL volumetric flask and dilute to volume with water.
\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.

[[Page 10757]]

 
\52\ Unless otherwise indicated, all EPA methods, excluding EPA Method 300.1, 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 U.S. 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 D6508-15, Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate
  Electrolyte. 2015. 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, 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 D6888-16 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 for
  the Examination of Water and Wastewater 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 BOD5 and CBOD5.
  Revision 1.2, October 2011. Hach Company. This method may be used to measure dissolved oxygen when performing the methods approved in Table IB of this
  section 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, ``Nitrate Reductase Nitrate-Nitrogen Analysis,'' Revision 9.0, March 2014, The Nitrate Elimination Co., Inc.
\74\ Timberline Instruments, LLC Method Ammonia-001, ``Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Conductivity Cell
  Analysis,'' June 2011, Timberline Instruments, LLC.
\75\ Hach Company Method 10206, ``Spectrophotometric Measurement of Nitrate in Water and Wastewater,'' Revision 2.1, January 2013, Hach Company.
\76\ Hach Company Method 10242, ``Simplified Spectrophotometric Measurement of Total Kjeldahl Nitrogen in Water and Wastewater,'' Revision 1.1, January
  2013, 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, National Council for Air and Stream Improvement, Inc.
\78\ The pH adjusted sample is to be adjusted to 7.6 for NPDES reporting purposes.
\79\ I-2057-85 U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Chap. A11989, Methods for Determination of Inorganic
  Substances in Water and Fluvial Sediments, 1989.
\80\ Methods I-2522-90, I-2540-90, and I-2601-90 U.S. Geological Survey Open-File Report 93-125, Methods of Analysis by the U.S. Geological Survey
  National Water Quality Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, 1993.
\81\ Method I-1472-97, U.S. Geological Survey Open-File Report 98-165, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments, 1998.
\82\ FIAlab Instruments, Inc. Method FIAlab 100, ``Determination of Inorganic Ammonia by Continuous Flow Gas Diffusion and Fluorescence Detector
  Analysis'', April 4, 2018, FIAlab Instruments, Inc.
\83\ MACHEREY-NAGEL GmbH and Co. Method 036/038 NANOCOLOR[supreg] COD LR/HR, ``Spectrophotometric Measurement of Chemical Oxygen Demand in Water and
  Wastewater'', Revision 1.5, May 2018, MACHEREY-NAGEL GmbH and Co. KG.
\84\ Please refer to the following applicable Quality Control Sections: Part 2000 Methods, Physical and Aggregate Properties 2020 (2021); Part 3000
  Methods, Metals, 3020 (2021); Part 4000 Methods, Inorganic Nonmetallic Constituents, 4020 (2022); Part 5000 Methods, and Aggregate Organic
  Constituents, 5020 (2022). These Quality Control Standards are available for download at www.standardmethods.org at no charge.
\85\ Each laboratory may establish its own control limits by performing at least 25 glucose-glutamic acid (GGA) checks over several weeks or months and
  calculating the mean and standard deviation. The laboratory may then use the mean  3 standard deviations as the control limit for future
  GGA checks. However, GGA acceptance criteria can be no wider than 198  30.5 mg/L for BOD5. GGA acceptance criteria for CBOD must be either
  198  30.5 mg/L, or the lab may develop control charts under the following conditions: dissolved oxygen uptake from the seed contribution
  is between 0.6-1.0 mg/L; control charts are performed on at least 25 GGA checks with three standard deviations from the derived mean; the RSD must not
  exceed 7.5%; and any single GGA value cannot be less than 150 mg/L or higher than 250 mg/L.
\86\ The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.

[[Page 10758]]

                                     Table IC--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
           Parameter \1\                     Method                EPA \2\ \7\       Standard methods \15\           ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene....................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
2. Acenaphthylene..................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
3. Acrolein........................  GC....................  603...................
                                     GC/MS.................  624.1,\4\ 1624B.......
4. Acrylonitrile...................  GC....................  603...................
                                     GC/MS.................  624.1,\4\ 1624B.......  .....................  .....................  O-4127-96.\13\
5. Anthracene......................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440B-2021...........  D4657-92 (98)........
6. Benzene.........................  GC....................  602...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
7. Benzidine.......................  Spectro-photometric...  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    1.
                                     GC/MS.................  625.1,\5\ 1625B.......  6410 B-2020..........
                                     HPLC..................  605...................
8. Benzo(a)anthracene..............  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
9. Benzo(a)pyrene..................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
10. Benzo(b)fluoranthene...........  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
11. Benzo(g,h,i)perylene...........  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
12. Benzo(k)fluoranthene...........  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  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-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
15. bis(2-Chloroethoxy) methane....  GC....................  611...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
16. bis(2-Chloroethyl) ether.......  GC....................  611...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
17. bis(2-Ethylhexyl) phthalate....  GC....................  606...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
18. Bromodichloromethane...........  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
19. Bromoform......................  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
20. Bromomethane...................  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
21. 4-Bromophenyl phenyl ether.....  GC....................  611...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
22. Carbon tetrachloride...........  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\

[[Page 10759]]

 
23. 4-Chloro-3-methyl phenol.......  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
24. Chlorobenzene..................  GC....................  601, 602..............  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
25. Chloroethane...................  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96.\13\
26. 2-Chloroethylvinyl ether.......  GC....................  601...................
                                     GC/MS.................  624.1, 1624B..........
27. Chloroform.....................  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
28. Chloromethane..................  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
29. 2-Chloronaphthalene............  GC....................  612...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
30. 2-Chlorophenol.................  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
31. 4-Chlorophenyl phenyl ether....  GC....................  611...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
32. Chrysene.......................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
33. Dibenzo(a,h)anthracene.........  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
34. Dibromochloromethane...........  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
35. 1,2-Dichlorobenzene............  GC....................  601, 602..............  6200 C-2020..........
                                     GC/MS.................  624.1, 1625B..........  6200 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96,\13\ O-
                                                                                                                                    4436-16.\14\
36. 1,3-Dichlorobenzene............  GC....................  601, 602..............  6200 C-2020..........
                                     GC/MS.................  624.1, 1625B..........  6200 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96.\13\
37. 1,4-Dichlorobenzene............  GC....................  601, 602..............  6200 C-2020..........
                                     GC/MS.................  624.1, 1625B..........  6200 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96,\13\ O-
                                                                                                                                    4436-16.\14\
38. 3,3'-Dichlorobenzidine.........  GC/MS.................  625.1, 1625B..........  6410 B-2020..........
                                     HPLC..................  605...................
39. Dichlorodifluoromethane........  GC....................  601...................
                                     GC/MS.................  ......................  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
40. 1,1-Dichloroethane.............  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
41. 1,2-Dichloroethane.............  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
42. 1,1-Dichloroethene.............  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
43. trans-1,2-Dichloroethene.......  GC....................  601...................  6200 C-2020..........

[[Page 10760]]

 
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
44. 2,4-Dichlorophenol.............  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
45. 1,2-Dichloropropane............  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
46. cis-1,3-Dichloropropene........  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
47. trans-1,3-Dichloropropene......  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
48. Diethyl phthalate..............  GC....................  606...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
49. 2,4-Dimethylphenol.............  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
50. Dimethyl phthalate.............  GC....................  606...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
51. Di-n-butyl phthalate...........  GC....................  606...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
52. Di-n-octyl phthalate...........  GC....................  606...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
53. 2, 4-Dinitrophenol.............  GC....................  604...................  6420 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........
54. 2,4-Dinitrotoluene.............  GC....................  609...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
55. 2,6-Dinitrotoluene.............  GC....................  609...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  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-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
58. Fluoranthene...................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
59. Fluorene.......................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
60. 1,2,3,4,6,7,8-Heptachloro-       GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
61. 1,2,3,4,7,8,9-Heptachloro-       GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
62. 1,2,3,4,6,7,8- Heptachloro-      GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzo-p-dioxin.                                                                                                                  16130-SSI.\16\
63. Hexachlorobenzene..............  GC....................  612...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
64. Hexachlorobutadiene............  GC....................  612...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96.\13\
65. Hexachlorocyclopentadiene......  GC....................  612...................
                                     GC/MS.................  625.1,\5\ 1625B.......  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96.\13\
66. 1,2,3,4,7,8-Hexachloro-          GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\

[[Page 10761]]

 
67. 1,2,3,6,7,8-Hexachloro-          GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
68. 1,2,3,7,8,9-Hexachloro-          GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
69. 2,3,4,6,7,8-Hexachloro-          GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
70. 1,2,3,4,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 p-dioxin.                                                                                                                          16130-SSI,\16\ G
                                                                                                                                    BHTYHGTGB B VB B5
                                                                                                                                    BV.
71. 1,2,3,6,7,8-Hexachloro-dibenzo-  GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 p-dioxin.                                                                                                                          16130-SSI.\16\
72. 1,2,3,7,8,9-Hexachloro-dibenzo-  GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 p-dioxin.                                                                                                                          16130-SSI.\16\
73. Hexachloroethane...............  GC....................  612...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96.\13\
74. Indeno(1,2,3-c,d) pyrene.......  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
75. Isophorone.....................  GC....................  609...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
76. Methylene chloride.............  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
77. 2-Methyl-4,6-dinitrophenol.....  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
78. Naphthalene....................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........
79. Nitrobenzene...................  GC....................  609...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  ......................  .....................  D4657-92 (98)........
80. 2-Nitrophenol..................  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
81. 4-Nitrophenol..................  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
82. N-Nitrosodimethylamine.........  GC....................  607...................
                                     GC/MS.................  625.1,\5\ 1625B.......  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
83. N-Nitrosodi-n-propylamine......  GC....................  607...................
                                     GC/MS.................  625.1,\5\ 1625B.......  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
84. N-Nitrosodiphenylamine.........  GC....................  607...................
                                     GC/MS.................  625.1,\5\ 1625B.......  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
85. Octachlorodibenzofuran.........  GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
                                                                                                                                    16130-SSI.\16\
86. Octachlorodibenzo-p-dioxin.....  GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
                                                                                                                                    16130-SSI.\16\
87. 2,2'-oxybis(1-chloropropane)     GC....................  611...................
 \12\ [also known as bis(2-Chloro-1-
 methylethyl) ether].
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  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-2020..........

[[Page 10762]]

 
89. PCB-1221.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
90. PCB-1232.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
91. PCB-1242.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
92. PCB-1248.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
93. PCB-1254.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
94. PCB-1260.......................  GC....................  608.3.................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    43; See footnote.\8\
                                     GC/MS.................  625.1.................  6410 B-2020..........
95. 1,2,3,7,8-Pentachloro-           GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
96. 2,3,4,7,8-Pentachloro-           GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
97. 1,2,3,7,8-Pentachloro-dibenzo-p- GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dioxin.                                                                                                                            16130-SSI.\16\
98. Pentachlorophenol..............  GC....................  604...................  6420 B-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    140.
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
99. Phenanthrene...................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
100. Phenol........................  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
101. Pyrene........................  GC....................  610...................
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
                                     HPLC..................  610...................  6440 B-2021..........  D4657-92 (98)........
102. 2,3,7,8-Tetrachloro-            GC/MS.................  1613B \10\............  .....................  .....................  ATM 16130,\15\ PAM
 dibenzofuran.                                                                                                                      16130-SSI.\16\
103. 2,3,7,8-Tetrachloro-dibenzo-p-  GC/MS.................  613, 625.1,\5a\ 1613B.  .....................  .....................  ATM 16130,\15\ PAM
 dioxin.                                                                                                                            16130-SSI.\16\
104. 1,1,2,2-Tetrachloroethane.....  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96.\13\
105. Tetrachloroethene.............  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
106. Toluene.......................  GC....................  602...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
107. 1,2,4-Trichlorobenzene........  GC....................  612...................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27 O-4127-96,\13\ O-
                                                                                                                                    4436-16.\14\
108. 1,1,1-Trichloroethane.........  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
109. 1,1,2-Trichloroethane.........  GC....................  601...................  6200 C-2020..........  .....................  See footnote,\3\ p.
                                                                                                                                    130.
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
110. Trichloroethene...............  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
111. Trichlorofluoromethane........  GC....................  601...................  6200 C-2020..........

[[Page 10763]]

 
                                     GC/MS.................  624.1.................  6200 B-2020..........  .....................  O-4127-96.\13\
112. 2,4,6-Trichlorophenol.........  GC....................  604...................  6420 B-2020..........
                                     GC/MS.................  625.1, 1625B..........  6410 B-2020..........  .....................  See footnote,\9\ p.
                                                                                                                                    27.
113. Vinyl chloride................  GC....................  601...................  6200 C-2020..........
                                     GC/MS.................  624.1, 1624B..........  6200 B-2020..........  .....................  O-4127-96,\13\ O-4436-
                                                                                                                                    16.\14\
114. Nonylphenol...................  GC/MS.................  ......................  .....................  D7065-17.............
115. Bisphenol A (BPA).............  GC/MS.................  ......................  .....................  D7065-17.............
116. p-tert-Octylphenol (OP).......  GC/MS.................  ......................  .....................  D7065-17.............
117. Nonylphenol Monoethoxylate      GC/MS.................  ......................  .....................  D7065-17.............
 (NP1EO).
118. Nonylphenol Diethoxylate        GC/MS.................  ......................  .....................  D7065-17.............
 (NP2EO).
119. Adsorbable Organic Halides      Adsorption and          1650 \11\.............
 (AOX).                               Coulometric Titration.
120. Chlorinated Phenolics.........  In Situ Acetylation     1653 \11\.............
                                      and GC/MS.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter ([micro]g/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. The
  standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at appendix B of this part,
  Definition and Procedure for the Determination of the Method Detection Limit. These methods are available at: https://www.epa.gov/cwa-methods as
  individual PDF files.
\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 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 quality control (QC) acceptance
  criteria in the pertinent method, analytical results for that parameter in the unspiked sample are suspect. The results should be reported but cannot
  be used to demonstrate regulatory compliance. If the method does not contain QC acceptance criteria, control limits of  three standard
  deviations around the mean of a minimum of five replicate measurements must be used. These quality control requirements also apply to the Standard
  Methods, ASTM Methods, and other methods cited.
\8\ 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 this part and at https://www.epa.gov/cwa-methods/approved-cwa-test-methods-organic-compounds.
\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
  of this chapter, 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.
\13\ Method O-4127-96, U.S. Geological Survey Open-File Report 97-829, Methods of analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of 86 volatile organic compounds in water by gas chromatography/mass spectrometry, including detections less than reporting
  limits, 1998, USGS.
\14\ Method O-4436-16 U.S. Geological Survey Techniques and Methods, book 5, chap. B12, Determination of heat purgeable and ambient purgeable volatile
  organic compounds in water by gas chromatography/mass spectrometry, 2016, USGS.
\15\ Please refer to the following Quality Control Section: Part 6000 Individual Organic Compounds, 6020 (2019) \16\ SGS AXYS Method ATM 16130,
  ``Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using Waters and Agilent Gas
  Chromatography-Tandem-Mass Spectrometry (GC/MS/MS), Revision 1.0, '' is available at: https://www.sgsaxys.com/wp-content/uploads/2022/09/SGS-AXYS-Method-16130-Rev-1.0.pdf.
\16\ Pace Analytical Method PAM-16130-SSI, ``Determination of 2,3,7,8-Substituted Tetra- through Octa-Chlorinated Dibenzo-p-Dioxins and Dibenzofurans
  (CDDs/CDFs) Using Shimadzu Gas Chromatography Mass Spectrometry (GC-MS/MS), Revision 1.1,'' is available at: www.pacelabs.com.

[[Page 10764]]

                                              Table ID--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
             Parameter                       Method             EPA \2\ \7\ \10\     Standard methods \15\           ASTM                  Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin..........................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-96     See footnote,\3\ p.
                                                                                                             (02).                  7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
2. Ametryn.........................  GC....................  507, 619..............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\9\
                                                                                                                                    O-3106-93; See
                                                                                                                                    footnote,\6\ p. S68.
                                     GC/MS.................  525.2, 625.1..........  .....................  .....................  See footnote,\14\ O-
                                                                                                                                    1121-91.
3. Aminocarb.......................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC..................  632...................
4. Atraton.........................  GC....................  619...................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.
                                     GC/MS.................  625.1.................
5. Atrazine........................  GC....................  507, 619, 608.3.......  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS.................  525.1, 525.2, 625.1...  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
6. Azinphos methyl.................  GC....................  614, 622, 1657........  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC-MS.................  625.1.................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
7. Barban..........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     GC/MS.................  625.1.................
8. [alpha]-BHC.....................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS.................  625.1 \5\.............  6410 B-2020..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
9. [beta]-BHC......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\8\
                                                                                                             96(02).                3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
10. [delta]-BHC....................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\8\
                                                                                                             96(02).                3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
11. [gamma]-BHC (Lindane)..........  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1 \5\.............  6410 B-2020..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
12. Captan.........................  GC....................  617, 608.3............  6630 B-2021..........  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7.
13. Carbaryl.......................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94, See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC..................  531.1, 632............
                                     HPLC/MS...............  553...................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS.................  625.1.................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
14. Carbophenothion................  GC....................  617, 608.3............  6630 B-2021..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
                                     GC/MS.................  625.1.................

[[Page 10765]]

 
15. Chlordane......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
16. Chloropropham..................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     GC/MS.................  625.1.................
17. 2,4-D..........................  GC....................  615...................  6640 B-2021..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
18. 4,4'-DDD.......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3105-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
19. 4,4'-DDE.......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
20. 4,4'-DDT.......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
21. Demeton-O......................  GC....................  614, 622..............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS.................  625.1.................
22. Demeton-S......................  GC....................  614, 622..............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS.................  625.1.................
23. Diazinon.......................  GC....................  507, 614, 622, 1657...  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\6\ p. S51.
                                     GC/MS.................  525.2, 625.1..........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
24. Dicamba........................  GC....................  615...................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    115.
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
25. Dichlofenthion.................  GC....................  622.1.................  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
26. Dichloran......................  GC....................  608.2, 617, 608.3.....  6630 B-2021..........  .....................  See footnote,\3\ p.
                                                                                                                                    7.
27. Dicofol........................  GC....................  617, 608.3............  .....................  .....................  See footnote,\4\ O-
                                                                                                                                    3104-83.
28. Dieldrin.......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
29. Dioxathion.....................  GC....................  614.1, 1657...........  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
30. Disulfoton.....................  GC....................  507, 614, 622, 1657...  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS.................  525.2, 625.1..........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
31. Diuron.........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.

[[Page 10766]]

 
                                     HPLC..................  632...................
                                     HPLC/MS...............  553...................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
32. Endosulfan I...................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M022).
                                     GC/MS.................  625.1 \5\.............  6410 B-2020..........  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
33. Endosulfan II..................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS.................  625.1 \5\.............  6410 B-2020..........  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
34. Endosulfan Sulfate.............  GC....................  617, 608.3............  6630 C-2021..........  .....................  See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
35. Endrin.........................  GC....................  505, 508, 617, 1656,    6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                              608.3.                                         96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  525.1, 525.2, 625.1     6410 B-2020..........
                                                              \5\.
36. Endrin aldehyde................  GC....................  617, 608.3............  6630 C-2021..........  .....................  See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
37. Ethion.........................  GC....................  614, 614.1, 1657......  .....................  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\6\
                                                                                                                                    p. S73.
                                     GC/MS.................  625.1.................  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
38. Fenuron........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
39. Fenuron-TCA....................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
40. Heptachlor.....................  GC....................  505, 508, 617, 1656,    6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                              608.3.                                         96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  525.1, 525.2, 625.1...  6410 B-2020..........
41. Heptachlor epoxide.............  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\6\ p. S73;
                                                                                                                                    See footnote,\8\
                                                                                                                                    3M0222.
                                     GC/MS.................  625.1.................  6410 B-2020..........
42. Isodrin........................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  .....................  See footnote,\4\ O-
                                                                                                                                    3104-83; See
                                                                                                                                    footnote,\6\ p. S73.
                                     GC/MS.................  625.1.................
43. Linuron........................  GC....................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     HPLC/MS...............  553...................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
                                     GC/MS.................  ......................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
44. Malathion......................  GC....................  614, 1657.............  6630 B-2021..........  .....................  See footnote,\3\ p.
                                                                                                                                    25; See footnote,\6\
                                                                                                                                    p. S51.
                                     GC/MS.................  625.1.................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
45. Methiocarb.....................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.

[[Page 10767]]

 
                                     HPLC..................  632...................
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
46. Methoxychlor...................  GC....................  505, 508, 608.2, 617,   6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                              1656, 608.3.                                   96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83; See
                                                                                                                                    footnote,\8\ 3M0222.
                                     GC/MS.................  525.1, 525.2, 625.1...  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
47. Mexacarbate....................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC..................  632...................
                                     GC/MS.................  625.1.................
48. Mirex..........................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7; See footnote,\4\
                                                                                                                                    O-3104-83.
                                     GC/MS.................  625.1.................
49. Monuron........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
50. Monuron-TCA....................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
51. Neburon........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
52. Parathion methyl...............  GC....................  614, 622, 1657........  6630 B-2021..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\3\
                                                                                                                                    p. 25.
                                     GC/MS.................  625.1.................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
53. Parathion ethyl................  GC....................  614...................  6630 B-2021..........  .....................  See footnote,\4\ page
                                                                                                                                    27; See footnote,\3\
                                                                                                                                    p. 25.
                                     GC/MS.................  ......................  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
54. PCNB...........................  GC....................  608.1, 617, 608.3.....  6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                                                                             96(02).                7.
55. Perthane.......................  GC....................  617, 608.3............  .....................  D3086-90, D5812-       See footnote,\4\ O-
                                                                                                             96(02).                3104-83.
56. Prometon.......................  GC....................  507, 619..............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS.................  525.2, 625.1..........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
57. Prometryn......................  GC....................  507, 619..............  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS.................  525.1, 525.2, 625.1...  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
58. Propazine......................  GC....................  507, 619, 1656, 608.3.  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS.................  525.1, 525.2, 625.1...
59. Propham........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.

[[Page 10768]]

 
60. Propoxur.......................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    94; See footnote,\6\
                                                                                                                                    p. S60.
                                     HPLC..................  632...................
61. Secbumeton.....................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.
                                     GC....................  619...................
62. Siduron........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
                                     HPLC/MS...............  ......................  .....................  .....................  See footnote,\12\ O-
                                                                                                                                    2060-01.
63. Simazine.......................  GC....................  505, 507, 619, 1656,    .....................  .....................  See footnote,\3\ p.
                                                              608.3.                                                                83; See footnote,\6\
                                                                                                                                    p. S68; See
                                                                                                                                    footnote,\9\ O-3106-
                                                                                                                                    93.
                                     GC/MS.................  525.1, 525.2, 625.1...  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
64. Strobane.......................  GC....................  617, 608.3............  6630 B-2021 & C-2021.  .....................  See footnote,\3\ p.
                                                                                                                                    7.
65. Swep...........................  TLC...................  ......................  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    104; See
                                                                                                                                    footnote,\6\ p. S64.
                                     HPLC..................  632...................
66. 2,4,5-T........................  GC....................  615...................  6640 B-2021..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
67. 2,4,5-TP (Silvex)..............  GC....................  615...................  6640 B-2021..........  .....................  See footnote,\3\ p.
                                                                                                                                    115; See
                                                                                                                                    footnote,\4\ O-3105-
                                                                                                                                    83.
68. Terbuthylazine.................  GC....................  619, 1656, 608.3......  .....................  .....................  See footnote,\3\ p.
                                                                                                                                    83; See footnote,\6\
                                                                                                                                    p. S68.
                                     GC/MS.................  ......................  .....................  .....................  See footnote,\13\ O-
                                                                                                                                    2002-01.
69. Toxaphene......................  GC....................  505, 508, 617, 1656,    6630 B-2021 & C-2021.  D3086-90, D5812-       See footnote,\3\ p.
                                                              608.3.                                         96(02).                7; See footnote; \8\
                                                                                                                                    See footnote,\4\ O-
                                                                                                                                    3105-83.
                                     GC/MS.................  525.1, 525.2, 625.1...  6410 B-2020..........
70. Trifluralin....................  GC....................  508, 617, 627, 1656,    6630 B-2021..........  .....................  See footnote,\3\ p.
                                                              608.3.                                                                7; See footnote,\9\
                                                                                                                                    O-3106-93.
                                     GC/MS.................  525.2, 625.1..........  .....................  .....................  See footnote,\11\ O-
                                                                                                                                    1126-95.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table IC of this
  section, where entries are listed by chemical name.
\2\ The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B,
  Definition and Procedure for the Determination of the Method Detection Limit, of this part.
\3\ Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater. September 1978. U.S. EPA. This EPA
  publication includes thin-layer chromatography (TLC) methods.
\4\ Methods for the Determination of Organic Substances in Water and Fluvial Sediments, Techniques of Water-Resources Investigations of the U.S.
  Geological Survey, Book 5, Chapter A3. 1987. USGS.
\5\ The method may be extended to include [alpha]-BHC, [gamma]-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
  Method 608 is the preferred method.
\6\ Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency, Supplement to the 15th Edition of Standard
  Methods for the Examination of Water and Wastewater.1981. American Public Health Association (APHA).
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608.3 and
  625.1 in accordance with procedures given in Section 8.2 of each of these methods. Additionally, each laboratory, on an on-going basis, must spike and
  analyze 10% of all samples analyzed with Method 608.3 or 5% of all samples analyzed with Method 625.1 to monitor and evaluate laboratory data quality
  in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits, the analytical results
  for that parameter in the unspiked sample are suspect. The results should be reported, but cannot be used to demonstrate regulatory compliance. These
  quality control requirements also apply to the Standard Methods, ASTM Methods, and other methods cited.
\8\ Organochlorine Pesticides and PCBs in Wastewater Using Empore\TM\ Disk. Revised October 28, 1994. 3M Corporation.
\9\ Method O-3106-93 is in Open File Report 94-37, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of
  Triazine and Other Nitrogen-Containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors. 1994. USGS.

[[Page 10769]]

 
\10\ EPA Methods 608.1, 608.2, 614, 614.1, 615, 617, 619, 622, 622.1, 627, and 632 are found in Methods for the Determination of Nonconventional
  Pesticides in Municipal and Industrial Wastewater, EPA 821-R-92-002, April 1992, U.S. EPA. EPA Methods 505, 507, 508, 525.1, 531.1 and 553 are in
  Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater, Volume II, EPA 821-R-93-010B, 1993, U.S. EPA. EPA
  Method 525.2 is in Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column Gas Chromatography/Mass
  Spectrometry, Revision 2.0, 1995, U.S. EPA. EPA methods 1656 and 1657 are in Methods for The Determination of Nonconventional Pesticides In Municipal
  and Industrial Wastewater, Volume I, EPA 821-R-93-010A, 1993, U.S. EPA. Methods 608.3 and 625.1 are available at: cwa-methods/approved-cwa-test-
  methods-organic-compounds.
\11\ Method O-1126-95 is in Open-File Report 95-181, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring. 1995.
  USGS.
\12\ Method O-2060-01 is in Water-Resources Investigations Report 01-4134, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of Pesticides in Water by Graphitized Carbon-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass
  Spectrometry. 2001. USGS.
\13\ Method O-2002-01 is in Water-Resources Investigations Report 01-4098, Methods of Analysis by the U.S. Geological Survey National Water Quality
  Laboratory--Determination of moderate-use pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass
  spectrometry. 2001. USGS.
\14\ Method O-1121-91 is in Open-File Report 91-519, Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination
  of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion
  monitoring. 1992. USGS.
\15\ Please refer to the following applicable Quality Control Section: Part 6000 Methods, Individual Organic Compounds 6020 (2019). These Quality
  Control Standards are available for download at www.standardmethods.org at no charge.

* * * * *
* * * * *

                                          Table IH--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
        Parameter and units                Method \1\                 EPA              Standard methods       AOAC, ASTM, USGS             Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Bacteria
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Coliform (fecal), number per 100  Most Probable Number    p. 132 \3\...........  9221 E-2014, 9221 F-
 mL.                                  (MPN), 5 tube, 3                               2014 \32\.
                                      dilution, or
                                     Membrane filter         p. 124 \3\...........  9222 D-2015 \26\.....  B-0050-85. \4\
                                      (MF),\2\ single step.
2. Coliform (total), number per 100  MPN, 5 tube, 3          p. 114 \3\...........  9221 B-2014..........
 mL.                                  dilution, or.
                                     MF,\2\ single step or   p. 108 \3\...........  9222 B-2015 \27\       B-0025-85. \4\
                                      two step.
                                     MF \2\ with enrichment  p. 111 \3\...........  9222 B.-2015. \27\
3. E. coli, number per 100 mL......  MPN,\5\ \7\ \13\        .....................  9221 B.3-2014/9221 F-
                                      multiple tube, or                              2014. \10\ \12\ \32\
                                     Multiple tube/multiple  .....................  9223 B-2016 \11\.....  991.15 \9\............  Colilert[supreg],\11\
                                      well, or.                                                                                     \15\ Colilert-
                                                                                                                                    18[supreg].\11\ \14\
                                                                                                                                    \15\
                                     MF,\2\ \5\ \6\ \7\ two  1103.2 \18\..........  9222 B-2015/9222 I-    D5392-93. \8\
                                      step, or.                                      2015,\17\ 9213 D-
                                                                                     2007.
                                     Single step...........  1603.1,\19\ 1604 \20\  .....................  ......................  m-
                                                                                                                                    ColiBlue24[supreg],\
                                                                                                                                    16\ KwikCount\TM\ EC
                                                                                                                                    \28\ \ 29\
4. Fecal streptococci, number per    MPN, 5 tube, 3          p. 139 \3\...........  9230 B-2013..........
 100 mL.                              dilution, or.
                                     MF,\2\ or.............  p. 136 \3\             9230 C-2013 \30\.....  B-0055-85. \4\
                                     Plate count...........  p. 143. \3\
5. Enterococci, number per 100 mL..  MPN,\5\ \7\ multiple    .....................  9230 D-2013..........  D6503-99 \8\..........  Enterolert[supreg]
                                      tube/multiple well,                                                                           \11\ \21\
                                      or
                                     MF \2\ \5\ \6\ \7\ two  1106.2 \22\..........  9230 C-2013 \30\.....  D5259-92. \8\
                                      step, or.
                                     Single step, or.......  1600.1 \23\..........  9230 C-2013. \30\
                                     Plate count...........  p. 143. \3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                        Protozoa
--------------------------------------------------------------------------------------------------------------------------------------------------------
6. Cryptosporidium.................  Filtration/IMS/FA.....  1622, \24\ 1623, \25\
                                                              1623.1. \25\ \31\
7. Giardia.........................  Filtration/IMS/FA.....  1623, \25\ 1623.1.
                                                              \25\ \31\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1H notes:
\1\ The method must be specified when results are reported.
\2\ A 0.45-[micro]m 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\ 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.
\6\ When the MF method has not been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may
  contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
  comparability of results.
\7\ 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.
\8\ Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. 2000, 1999, 1996. ASTM International.
\9\ Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. 1995. AOAC International.
\10\ The multiple-tube fermentation test is used in 9221B.3-2014. 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.
\11\ These tests are collectively known as defined enzyme substrate tests.

[[Page 10770]]

 
\12\ After prior enrichment in a presumptive medium for total coliform using 9221B.3-2014, 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-2014. Commercially available EC-MUG media or EC media
  supplemented in the laboratory with 50 [micro]g/mL of MUG may be used.
\13\ 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[supreg] may be enumerated with
  the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg]/2000, and the MPN calculated from the table provided by the manufacturer.
\14\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
  within 18 h of incubation at 35 [deg]C, rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\15\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
  Laboratories Inc.
\16\ A description of the mColiBlue24[supreg] test may be obtained from Hach Company.
\17\ Subject coliform positive samples determined by 9222B-2015 or other membrane filter procedure to 9222I-2015 using NA-MUG media.
\18\ Method 1103.2: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC), [in draft as
  of 2023]. US EPA.
\19\ Method 1603.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified
  mTEC), [in draft as of 2023]. US EPA.
\20\ Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI
  Medium), EPA 821-R-02-024. September 2002. US EPA.
\21\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories Inc.
\22\ Method 1106.2: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA), [in draft as of 2023]. US EPA.
\23\ Method 1600.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI), [in draft as of
  2023]. US EPA.
\24\ Method 1622 uses a filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
  concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
  Method 1622: Cryptosporidium in Water by Filtration/IMS/FA, EPA-821-R-05-001. December 2005. US EPA.
\25\ Methods 1623 and 1623.1 use a filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence
  assay to determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous
  detection of Cryptosporidium and Giardia oocysts and cysts. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA-821-R-05-002.
  December 2005. US EPA. Method 1623.1: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. EPA 816-R-12-001. January 2012. US EPA.
\26\ On a monthly basis, at least ten blue colonies from positive samples must be verified using Lauryl Tryptose Broth and EC broth, followed by count
  adjustment based on these results; and representative non-blue colonies should be verified using Lauryl Tryptose Broth. Where possible, verifications
  should be done from randomized sample sources.
\27\ On a monthly basis, at least ten sheen colonies from positive samples must be verified using Lauryl Tryptose Broth and brilliant green lactose bile
  broth, followed by count adjustment based on these results; and representative non-sheen colonies should be verified using Lauryl Tryptose Broth.
  Where possible, verifications should be done from randomized sample sources.
\28\ A description of KwikCount\TM\ EC may be obtained from Micrology Laboratories LLC.
\29\ Approved for the analyses of E. coli in freshwater only.
\30\ Verification of colonies by incubation of BHI agar at 10  0.5 [deg]C for 48  3 h is optional. As per the Errata to the 23rd
  Edition of Standard Methods for the Examination of Water and Wastewater ``Growth on a BHI agar plate incubated at 10  0.5 [deg]C for 48
   3 h is further verification that the colony belongs to the genus Enterococcus.''
\31\ Method 1623.1 includes updated acceptance criteria for IPR, OPR, and MS/MSD and clarifications and revisions based on the use of Method 1623 for
  years and technical support questions.
\32\ 9221 F.2-2014 allows for simultaneous detection of E. coli and thermotolerant fecal coliforms by adding inverted vials to EC-MUG; the inverted
  vials collect gas produced by thermotolerant fecal coliforms.

    (b) The material listed in this paragraph (b) is incorporated by 
reference into this section with the approval of the Director of the 
Federal Register under 5 U.S.C. 552(a) and 1 CFR part 51. All approved 
material is available for inspection at the EPA and at the National 
Archives and Records Administration (NARA). Contact the EPA at: EPA's 
Water Docket, EPA West, 1301 Constitution Avenue NW, Room 3334, 
Washington, DC 20004; telephone: 202-566-2426; email: [email protected]. For information on the availability of this 
material at NARA, visit www.archives.gov/federal-register/cfr/ibr-locations.html or email [email protected]. The material may be 
obtained from the following sources in this paragraph (b).
* * * * *
    (8) * * *
    (ii) Method 1103.2: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar 
(Modified mTEC). [in draft as of 2023]. EPA Table IH, Note 18.
    (iii) Method 1106.2: Enterococci in Water by Membrane Filtration 
Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). [in draft as of 
2023]. Table IH, Note 22.
    (iv) Method 1600.1: Enterococci in Water by Membrane Filtration 
Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). [in 
draft as of 2023]. EPA. Table 1A, Note 24; Table IH, Note 23.
    (v) Method 1603.1: Escherichia coli (E. coli) in Water by Membrane 
Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar 
(Modified mTEC). [in draft as of 2023]. EPA. Table IA, Note 21; Table 
IH, Note 19.
* * * * *
    (10) * * *
    (i) Standard Methods for the Examination of Water and Wastewater. 
14th Edition, 1975. Table IB, Notes 27 and 86.
* * * * *
    (viii) 2120, Color. 2021. Table IB.
    (ix) 2130, Turbidity. 2020. Table IB.
    (x) 2310, Acidity. 2020. Table IB.
    (xi) 2320, Alkalinity. 2021. Table IB.
    (xii) 2340, Hardness. 2021. Table IB.
    (xiii) 2510, Conductivity. 2021. Table IB.
    (xiv) 2540, Solids. 2020. Table IB.
* * * * *
    (xvi) 3111, Metals by Flame Atomic Absorption Spectrometry. 2019. 
Table IB.
    (xvii) 3112, Metals by Cold-Vapor Atomic Absorption Spectrometry. 
2020. Table IB.
    (xviii) 3113, Metals by Electrothermal Atomic Absorption 
Spectrometry. 2020. Table IB.
    (xix) 3114, Arsenic and Selenium by Hydride Generation/Atomic 
Absorption Spectrometry. 2020, Table IB.
    (xx) 3120, Metals by Plasma Emission Spectroscopy. 2020. Table IB.
    (xxi) 3125, Metals by Inductively Coupled Plasma-Mass Spectrometry. 
2020. Table IB.
    (xxii) 3500-Al, Aluminum. 2020. Table IB.
    (xxiii) 3500-As, Arsenic. 2020. Table IB.
    (xxiv) 3500-Ca, Calcium. 2020. Table IB.
    (xxv) 3500-Cr, Chromium. 2020. Table IB.
    (xxvi) 3500-Cu, Copper. 2020. Table IB.
* * * * *
    (xxviii) 3500-Pb, Lead. 2020. Table IB.
    (xxix) 3500-Mn, Manganese. 2020. Table IB.
    (xxx) 3500-K, Potassium. 2020. Table IB.
    (xxxi) 3500-Na, Sodium. 2020. Table IB.
* * * * *
    (xxxiii) 3500-Zn, Zinc. 2020. Table IB.
    (xxxiv) 4110, Determination of Anions by Ion Chromatography. 2020. 
Table IB.
    (xxxv) 4140, Inorganic Anions by Capillary Ion Electrophoresis. 
2020. Table IB.
* * * * *

[[Page 10771]]

    (xxxvii) 4500 Cl-, Chloride. 2021. Table IB.
* * * * *
    (xxxix) 4500-CN-, Cyanide. 2021. Table IB.
    (xl) 4500-F-, Fluoride. 2021. Table IB.
    (xli) 4500-H\+\, pH Value. 2021. Table IB.
    (xlii) 4500-NH3, Nitrogen (Ammonia). 2021. Table IB.
    (xliii) 4500-NO2-, Nitrogen (Nitrite). 2021. 
Table IB.
    (xliv) 4500-NO3-, Nitrogen (Nitrate). 2019. 
Table IB.
    (xlv) 4500-N(org), Nitrogen (Organic). 2021. Table IB.
    (xlvi) 4500-O, Oxygen (Dissolved). 2021. Table IB.
    (xlvii) 4500-P, Phosphorus. 2021. Table IB.
    (xlviii) 4500-SiO2, Silica. 2021. Table IB.
    (xlix) 4500-S2-, Sulfide. 2021. Table IB.
    (l) 4500-SO32-, Sulfite. 2021. Table IB.
    (li) 4500-SO42-, Sulfate. 2021. Table IB.
* * * * *
    (lv) 5520, Oil and Grease. 2021. Table IB.
    (lvi) 5530, Phenols. 2021. Table IB.
    (lvii) 5540, Surfactants. 2021. Table IB.
    (lviii) 6200, Volatile Organic Compounds. 2020. Table IC.
    (lix) 6410, Extractable Base/Neutrals and Acids. 2020. Tables IC 
and ID.
    (lx) 6420, Phenols. 2020. Table IC.
    (lxi) 6440, Polynuclear Aromatic Hydrocarbons. 2021. Table IC.
    (lxii) 6630, Organochlorine Pesticides. 2021. Table IC.
    (lxiii) 6640, Acidic Herbicide Compounds. 2021. Table IC.
* * * * *
    (lxvii) 9221, Multiple-Tube Fermentation Techniques for Members of 
the Coliform Group. 2014. Table IA, Notes 12, 14 and 33; Table IH, 
Notes 10, 12 and 32.
* * * * *
    (15) * * *
    (xi) ASTM D888-18, Standard Test Methods for Dissolved Oxygen in 
Water. May 2018. Table IB.
* * * * *
    (xx) ASTM D1293-18, Standard Test Methods for pH of Water. January 
2018. Table IB.
* * * * *
    (xxx) ASTM D1976-20, Standard Test Method for Elements in Water by 
Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy. June 
2020. Table IB.
* * * * *
    (xxxii) ASTM D2330-20, Standard Test Method for Methylene Blue 
Active Substances. February 2020. Table 1B.
* * * * *
    (lix) ASTM D5907-18, Standard Test Methods for Filterable Matter 
(Total Dissolved Solids) and Nonfilterable Matter (Total Suspended 
Solids) in Water. May 2018. Table IB.
* * * * *
    (lxv) ASTM D7237-18, Standard Test Method for Free Cyanide with 
Flow Injection Analysis (FIA) Utilizing Gas Diffusion Separation and 
Amperometric Detection. January 2019. Table IB.
    (lxvi) ASTM D7284-20, Standard Test Method for Total Cyanide in 
Water by Micro Distillation followed by Flow Injection Analysis with 
Gas Diffusion Separation and Amperometric Detection. August 2020. Table 
IB.
    (lxvii) ASTM D7365-09a (Reapproved 2015), Standard Practice for 
Sampling, Preservation and Mitigating Interferences in Water Samples 
for Analysis of Cyanide. August 2015. Table II, Notes 5 and 6.
* * * * *
    (lxix) ASTM D7573-18a\e1\, Standard Test Method for Total Carbon 
and Organic Carbon in Water by High Temperature Catalytic Combustion 
and Infrared Detection, January 2019. Table IB.
* * * * *
    (33) Pace Analytical Services, LLC, 1800 Elm Street SE, 
Minneapolis, MN 55414. Telephone: 612-656-2240.
    (i) PAM-16130-SSI, Determination of 2,3,7,8-Substituted Tetra- 
through Octa-Chlorinated Dibenzo-p-Dioxins and Dibenzofurans (CDDs/
CDFs) Using Shimadzu Gas Chromatography Mass Spectrometry (GC-MS/MS), 
Revision 1.1, May 20, 2022. Table IC, Note 17.
    (ii) [Reserved]
    (34) SGS AXYS Analytical Services, Ltd., 2045 Mills Road, Sidney, 
British Columbia, Canada, V8L 5X2. Telephone: 1-888-373-0881.
    (i) ATM 16130, Determination of 2,3,7,8-Substituted Tetra- through 
Octa-Chlorinated Dibenzo-p-Dioxins and Dibenzofurans (CDDs/CDFs) Using 
Waters and Agilent Gas Chromatography-Tandem-Mass Spectrometry (GC/MS/
MS)., Revision 1.0, August 2020. Table IC, Note 16
    (ii) [Reserved]
* * * * *
    (e) * * *

   Table II--Required Containers, Preservation Techniques, and Holding
                                  Times
------------------------------------------------------------------------
 
-------------------------------------------------------------------------
 
                              * * * * * * *
------------------------------------------------------------------------
 * * * * * * *
\5\ ASTM D7365-09a (15) specifies treatment options for samples
  containing oxidants (e.g., chlorine) for cyanide analyses. Also,
  Section 9060A of Standard Methods for the Examination of Water and
  Wastewater (23rd edition) addresses dechlorination procedures for
  microbiological analyses.

* * * * *
[FR Doc. 2023-02391 Filed 2-17-23; 8:45 am]
BILLING CODE 6560-50-P