[Federal Register Volume 60, Number 201 (Wednesday, October 18, 1995)]
[Proposed Rules]
[Pages 53988-54006]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 95-25775]




[[Page 53987]]

_______________________________________________________________________

Part III





Environmental Protection Agency





_______________________________________________________________________



40 CFR Part 136



Guidelines Establishing Test Procedures for the Analysis of Pollutants: 
New Methods; Proposed Rule

  Federal Register / Vol. 60, No. 201 / Wednesday, October 18, 1995 / 
Proposed Rules   

[[Page 53988]]


ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 136

[FRL-5308-4]


Guidelines Establishing Test Procedures for the Analysis of 
Pollutants: New Methods

AGENCY: Environmental Protection Agency (EPA).

ACTION: Proposed rule and request for comment.

-----------------------------------------------------------------------

SUMMARY: Under the Clean Water Act, Section 304(h), EPA proposes to 
amend its list of approved analytical techniques by adding new or 
revised test procedures for certain metal and inorganic chemical 
pollutants, by adding method citations to Table IB and by amending the 
incorporation by reference section of the regulation accordingly.
    EPA is also proposing to substitute reagents that are more 
environmentally friendly for certain hazardous and toxic chemical 
reagents currently used in certain approved methods.
    In addition, EPA is proposing to withdraw approval of certain 
outdated or little used analytical methods, as well as, certain methods 
that require the use of hazardous or toxic reagents. For each method 
that is proposed for withdrawal, one or more commonly used methods have 
been previously approved.
    Comments are requested on this proposed rulemaking. After 
considering comments received in response to this proposal, EPA will 
promulgate a final rule.
    This action amends guidelines establishing test procedures for the 
analysis of pollutants by adding clarifying notes to lists of approved 
test procedures, by adding and updating certain method citations in 
Tables IB and IC, and by amending the incorporation by reference 
section of the regulation accordingly.

DATES: Comments on the proposed amendments will be accepted until 
December 18, 1995.

ADDRESSES: Send written comments to the 304(h) Docket Clerk (Ben 
Honaker), Water Docket (MC-4101), U.S. Environmental Protection Agency, 
401 M Street, SW., Washington, DC 20460. Please submit any references 
cited in your comments. EPA would appreciate an original and three 
copies of your comments and enclosures (including references). 
Commenters who want EPA to acknowledge receipt of their comments should 
enclose a self-addressed, stamped envelope. No facsimiles (faxes) will 
be accepted because EPA cannot assure that they will be submitted to 
the Water Docket.
    The supporting materials are available for review at the Water 
Docket at the address above. For access to Docket Materials, call (202) 
260-3027 between 9 am and 3:30 pm for an appointment.

FOR FURTHER INFORMATION CONTACT: Mr. James E. Longbottom, Aquatic 
Research Division, National Exposure Research Laboratory, Office of 
Research and Development, U.S. Environmental Protection Agency, 
Cincinnati, Ohio 45268. Telephone number: (513) 569-7308.

SUPPLEMENTARY INFORMATION:
    Materials in the public docket include:
     ``Methods for the Determination of Metals in Environmental 
Samples'' Supplement I, EPA-600/R-94/111, May 1994.
     ``Methods for the Determination of Inorganic Substances in 
Environmental Samples'', EPA-600/R-93/100, August 1993.
     ``Determination of Trace Elements in Water by Inductively 
Coupled Plasma-Mass Spectrometry: Collaborative Study'', Journal of 
AOAC-International, 77, pp. 1004-1023, 1994.
     ``Determination of Inorganic Anions in Water by Ion 
Chromatography: Collaborative Study'', Journal of AOAC-International, 
77, pp. 1253-1263, 1994.
     ``Ion Chromatographic Method for Dissolved Hexavalent 
Chromium in Drinking Water, Ground Water, and Industrial Wastewater 
Effluents: Collaborative Study'', Journal of AOAC-International, 77, 
pp. 994-1004, 1994.
     ``Low-level Chlorine Analysis by Amperometric Titration'', 
Journal of the Water Pollution Control Federation, 51, pp. 2636-2640, 
1979.
    A copy of the first two items can also be obtained from EPA through 
a facsimile request to the Chemistry Research Branch, Aquatic Research 
Division, Cincinnati, Ohio, on (513) 569-7757.

I. Authority

    This regulation is proposed under authority of sections 301, 304(h) 
and 501(a) of the Clean Water Act, 33 U.S.C. 1251 et seq. (the Federal 
Water Pollution Control Act Amendments of 1972 as amended) (the 
``Act''). Section 301 prohibits the discharge of any pollutant into 
navigable waters unless the discharge complies with a NPDES permit, 
issued under Section 402 of the Act. Section 304(h) of the Act requires 
the Administrator of the EPA to ``promulgate guidelines establishing 
test procedures for the analysis of pollutants that shall include the 
factors which must be provided in any certification pursuant to section 
401 of this Act or permit application pursuant to section 402 of this 
Act''. Section 501(a) of the Act authorizes the Administrator to 
``prescribe such regulations as are necessary to carry out his 
functions under this Act''.
    The use of approved test procedures or approved alternate 
procedures is required whenever the waste constituent specified is 
required to be measured for: an NPDES permit application; discharge 
monitoring reports; state certification; and other requests from the 
permitting authority for quantitative or qualitative effluent data. Use 
of approved test procedures is also required for the expression of 
pollutant amounts, characteristics, or properties in effluent 
limitations guidelines and standards of performance and pretreatment 
standards, unless otherwise specifically noted or defined.

II. Regulatory Background

    The CWA establishes two principal bases for effluent limitations. 
First, existing discharges are required to meet technology-based 
effluent limitations. New source discharges must meet new source 
performance standards based on the best demonstrated technology-based 
controls. Second, where necessary, additional requirements are imposed 
to assure attainment and maintenance of water quality standards 
established by the States under Section 303 of the CWA. In establishing 
or reviewing NPDES permit limits, EPA must ensure that permitted 
discharges will not cause or contribute to a violation of water quality 
standards, including designated water uses.
    For use in permit applications, discharge monitoring reports, and 
state certification and to ensure compliance with effluent limitations, 
standards of performance, and pretreatment standards, EPA has 
promulgated regulations providing nationally-approved testing 
procedures at 40 CFR Part 136. Test procedures have previously been 
approved for 262 different parameters. Those procedures apply to the 
analysis of inorganic (metal, non-metal, mineral) and organic chemical 
(including pesticides), radiological, biological, nutrient, demand, 
residue, and physical parameters.
    Additionally, some particular industries may discharge pollutants 
for which test procedures have not been proposed and approved under 40 
CFR Part 136. Under 40 CFR 122.41 permit writers may impose monitoring 

[[Page 53989]]
requirements and establish test methods for pollutants for which no 
approved Part 136 method exists. 40 CFR 122.41(j) (4). EPA may also 
approve additional test procedures when establishing industry-wide 
technology-based effluent limitations guidelines and standards as 
described at 40 CFR 401.13.
    The procedures for approval of alternate test procedures (ATPs) are 
described at 40 CFR 136.4 and 136.5. Under these procedures the 
Administrator may approve alternate test procedures for nationwide use 
which are developed and proposed by any person. 40 CFR 136.4 (a). 
Persons wishing to use such alternate procedures, must apply to the 
State or Regional EPA permitting office [for limited approval under 
136.4 (b)], and to the Director of the Environmental Monitoring Systems 
Laboratory in Cincinnati [for nationwide approval under 136.4 (d)]. As 
specified below, today's proposed rule would approve additional 
nationwide test procedures for certain metals, anions, Cr(VI) and VOCs 
in wastewater and related samples.

III. Summary of Proposed Methods

    The proposed methods have been reviewed by appropriate members of 
and written in the EPA Environmental Monitoring Management Council 
Format.
    The methods proposed for addition include new methods for: 
preparation of samples for metals analysis, inductively coupled plasma/
mass spectrometry (ICP/MS), a stabilized temperature graphite furnace 
atomic absorption (STGFAA) method for metals, and ion chromatography 
(IC) methods for anions and for hexavalent chromium [Cr(VI)]. A revised 
EPA inductively coupled plasma atomic emission spectrometry (ICP-AES) 
method for metals to replace the currently approved method, and a low-
level extension of the approved method for the determination of low 
level total residual chlorine are also being proposed.
    Methods 200.7, 200.8, and 200.9 were approved for use in EPA's 
drinking water programs at 40 CFR Part 141.23(k)(1) on December 5, 1994 
(59 FR 62466). When the methods proposed today are promulgated at 40 
CFR Part 136 for use in EPA's wastewater programs, these three methods 
will be conformed for the two programs.
    Although not part of today's proposal, the Agency's Environmental 
Monitoring Management Council (EMMC) will soon propose integrated 
methods for citation in several regulations, including those at Part 
136. The methods include a graphite furnace atomic absorption 
spectrometry method for certain metals and an inductively coupled 
plasma atomic emissions spectrometry method for metals. These methods 
may be included in the final rule for today's proposal.
    In the interest of pollution prevention, EPA is proposing to 
replace mercuric sulfate with copper sulfate in the total Kjeldahl 
nitrogen methods and to permit the substitution of the AMCO-AEPA-1 
Standard for the formazin standard in the turbidity method. Replacement 
of these two reagents would remove hazardous or potentially 
carcinogenic chemicals from use in EPA approved methods.

A. Sample Preparation for Total Recoverable Elements

    EPA is proposing a new broad-purpose digestion procedure for total 
recoverable elements. It has the advantage of being compatable with 
several of the approved measurement techniques, which will allow 
laboratories to achieve some cost savings by reducing preparations and 
increasing flexibility in choosing approved analytical techniques after 
digestion. This preparation procedure is a variation of the procedures 
given in the previously approved EPA 200 Series Methods for ``total 
recoverable'' metals published in ``Methods for Chemical Analysis of 
Water and Wastes''. It utilizes the same acid combination (nitric + 
hydrochloric) as the previous ``total recoverable'' procedures, but the 
acid concentration has been modified by lowering the amount of 
hydrochloric acid.
    This sample preparation procedure has been incorporated into three 
EPA Methods proposed today, including, a May 1994 revision of the 
approved ICP/AES Method 200.7, a new measurement technology ICP/MS 
Method 200.8, and a stabilized temperature graphite furnace automatic 
absorption (GFAA) method (Method 200.9). In addition, EPA has prepared 
a stand-alone version of the digestion procedure: Method 200.2 ``Sample 
Preparation Procedure for Spectrochemical Determination of Total 
Recoverable Elements''. EPA proposes to permit the substitution of 
Method 200.2 for the digestion procedure in certain non-EPA approved 
direct aspiration flame atomic absorption procedures. The digestion 
procedure has been tested on various matrices using determinative 
methods 200.7, 200.8 and 200.9 and has been found comparable to 
previously approved NPDES preparation procedures. Method 200.2 was also 
validated through interlaboratory testing in the joint EPA/AOAC 
International study of Method 200.8. Each of the new EPA procedures 
includes: a list of elements to which it applies, sample preservation 
practices, and preparation conditions.
    EPA proposes to withdraw the EPA AA direct aspiration and AA 
furnace methods contained in ``Methods for Chemical Analysis of Water 
and Wastes''. The methods are out of date and lack many of the 
necessary instructions included in more recently produced EPA methods. 
The remaining approved non-EPA methods for AA direct aspiration are 
sufficiently identical to the withdrawn methods as to result in no 
impact on the regulated community. The EPA furnace methods are being 
replaced by EPA Method 200.9. Appendix D to this regulation, which 
contains the interlaboratory measures of precision and accuracy for the 
EPA methods that are being withdrawn, would also be removed by this 
proposal.

B. Elemental Analysis by ICP/AES

    The EPA proposes to approve the May 1994 revision of Method 200.7, 
``Determination of Metals and Trace Elements in Water and Wastes by 
Inductively Coupled Plasma-Atomic Emission Spectrometry'' and to cite 
the revised method by reference. Accordingly, Appendix C to 40 CFR Part 
136 would be deleted. The May 1994 edition of the method has been 
demonstrated to produce precision and recovery for the applicable 
elements that is equal to or better than that achieved by the currently 
approved edition and published in Table 4 of Appendix C. The procedure 
includes: A list of elements to which it applies, sample collection 
practices, preparation conditions, and quality control practices. The 
EMMC inductively coupled plasma-atomic emission spectrometry method 
being proposed elsewhere is proposed to be interchangeable with Method 
200.7 for the purposes of this regulation.

C. Elemental Analysis by ICP/MS

    The Agency is proposing a new multielement test procedure, ICP/MS, 
Method 200.8 ``Determination of Trace Elements in Waters and Wastes by 
Inductively Coupled Plasma-Mass Spectrometry'' for the detection and 
quantification of 20 metals in aqueous samples. Sample material in 
solution is introduced by pneumatic nebulization into a radio-frequency 
plasma where energy transfer processes cause desolvation, atomization 
and ionization. The ions are extracted from the plasma through a 
differentially pumped vacuum interface and separated on the basis of 
their mass-to-charge ratio by a 

[[Page 53990]]
quadrupole mass spectrometer having a minimum resolution capability of 
1 amu peak width at 5% peak height. The ions transmitted through the 
quadrupole are registered by an electron multiplier or Faraday detector 
and the ion information processed by a data handling system. 
Interferences relating to the technique must be identified and results 
must be corrected accordingly. Such corrections must include 
compensation for isobaric elemental interferences and interferences 
from polyatomic ions derived from the plasma gas, reagents or sample 
matrix. Instrumental drift, as well as suppressions or enhancements of 
instrument response caused by the sample matrix, must be corrected by 
the use of internal standardization.
    The Agency developed ICP/MS Method 200.8 under a contract and in 
cooperation with AOAC International jointly conducted an 
interlaboratory validation study of the method. This method (May 1994) 
represents the current state-of-the-art for the determination of metals 
in wastewater and water related media. The method description includes 
a list of the elements to which the method applies, sample collection 
practices, recommended analytical conditions, quality control 
practices, instrumental and method detection limits, and performance 
criteria based on the interlaboratory study data.
    AOAC-International has approved and published this ICP/MS method 
along with the study results as AOAC-International Method 993.14. The 
same method is in the final stages of the ASTM consensus process. EPA 
proposes to approve the AOAC-International method, as well as, consider 
approval of the ASTM ICP/MS Method if full ASTM Society acceptance is 
achieved prior to final EPA rulemaking.

D. Elemental Analysis by Stabilized Temperature Platform GFAA

    The May 1994 Revision of Method 200.9 ``Determination of Trace 
Metals by Stabilized Temperature Graphite Furnace Atomic Absorption'' 
is being proposed as a replacement for the currently approved EPA 
furnace methods. Method 200.9 determines elements by stabilized 
temperature graphite furnace atomic absorption (STGFAA). In STGFAA, the 
sample and required matrix modifier are first pipetted onto the 
platform or a device which provides delayed atomization. The sample is 
then dried at a relatively low temperature (120 deg.C) to 
avoid spattering. Once dried, the sample is normally pretreated in a 
char or ashing step which is designed to minimize the interference 
effects caused by the concomitant sample matrix. After the char step, 
the furnace is allowed to cool prior to atomization. The atomization 
cycle is characterized by rapid heating of the furnace to a temperature 
where the metal (analyte) is atomized from the pyrolytic graphite 
surface. The resulting atomic cloud absorbs the element specific atomic 
emission produced by a hollow cathode lamp or a electrodeless discharge 
lamp.
    Because the resulting absorbance usually has a nonspecific 
component associated with the actual analyte absorbance, an 
instrumental background correction device is necessary to subtract from 
the total signal the component which is nonspecific to the analyte. In 
the absence of interferences, the background corrected absorbance is 
directly related to the concentration of the analyte. Interferences 
relating to suppression or enhancement of instrument response caused by 
the sample matrix, must be corrected by the method of standard 
addition.
    The method description includes a list of elements to which the 
method applies, sample collection practices, recommended analytical 
conditions, quality control practices, method detection limits and 
performance criteria based on single laboratory study data. The EMMC 
furnace atomic absorption method being proposed elsewhere is proposed 
to be interchangeable with Method 200.9 for the purposes of this 
regulation.

E. Anions by Ion Chromatography

    EPA developed IC Method 300.0 for the following anions: Bromide, 
chloride, fluoride, nitrate-N, nitrite-N, ortho-phosphate, and sulfate. 
Using IC, a water sample is injected into a stream of carbonate-
bicarbonate eluent and passed through a series of ion exchangers. The 
anions of interest are separated on the basis of their relative 
affinities for a low capacity, strongly basic anion exchanger (guard 
and separator columns). The separated anions are directed through a 
hollow fiber cation exchanger membrane (fiber suppressor) or 
micromembrane suppressor bathed in continuously flowing strongly acid 
solution (regenerant solution). In the suppressor the separated anions 
are converted to their highly conductive acid forms and the carbonate-
bicarbonate eluent is converted to weakly conductive carbonic acid. The 
separated anions in their acid forms are measured by conductivity. They 
are identified on the basis of retention time as compared to reference 
standards. Quantitation is by measurement of peak area or peak height.
    EPA, in cooperation with ASTM Committee D-19 on Water, has 
conducted an interlaboratory validation study of EPA method 300.0 ``The 
Determination of Inorganic Anions in Water by Ion Chromatography'', 
August 1993. The method represents current state-of-the-art for 
determination of the anions listed above. The method description 
includes: Sample collection practices, recommended analytical 
conditions, quality control practices and estimated detection limits 
for the applicable analytes and performance criteria based on the 
interlaboratory study data. ASTM, Standard Methods, and AOAC-
International have approved the method under their consensus systems 
and have published the method in their Books of Standards. EPA also 
proposes to approve the ASTM Method D-4327, as well as, Method 4110 B 
published in the 18th edition of ``Standard Methods for the Examination 
of Water and Wastewater'' (SMEWW) and AOAC-International Method 993.30 
all of which were derived from EPA Method 300.0.

F. Cr (VI) by Ion Chromatography

    Using the IC Cr(VI) Method (Method 218.6), an aqueous sample is 
filtered through a 0.45 m filter and the filtrate is adjusted 
to a pH of 9 to 9.5 with a buffer solution. A measured volume of sample 
(50-250 l) is introduced into the ion chromatograph. A guard 
column is employed to remove organics from the sample prior to 
separation of Cr(VI) as CrO4-2 on an anion exchange separator 
column. Cr(VI) is determined by post column derivatization with 
diphenylcarbazide and passing through a low-volume flow-through cell 
and detection of the colored complex with a visible lamp detector at 
530 nm.
    EPA, in cooperation with ASTM Committee D-19 on Water, has 
conducted an interlaboratory validation study of EPA Method 218.6 
``Determination of Dissolved Hexavalent Chromium in Drinking Water, 
Ground Water, and Industrial Wastewater Effluents by Ion 
Chromatography''. The method description includes: Sample collection 
practices, recommended analytical conditions, quality control practices 
and method detection limits for Cr(VI), as well as performance criteria 
based on the interlaboratory study data.
    ASTM, Standard Methods, and AOAC-International have approved this 
method as a standard test method under their consensus systems and have 
published it in their manuals of methods. EPA also proposes to approve 
the ASTM Method D-5257, Standard Methods Method 3500-Cr E, and 

[[Page 53991]]
Method 993.23 from the AOAC-International Official Methods of Analysis, 
16th Edition. All three of these methods were derived from EPA Method 
218.6.

G. Method for Determination of Low Level Residual Chlorine

    EPA is proposing to additionally approve SMEWW, Method 4500-Cl E 
for the detection and quantification of low levels of chlorine in 
water. This method is a minor modification of the approved amperometric 
Method 4500-Cl D and is capable of measuring down to 10 g/L 
chlorine. Federal and State permitting authorities have requested such 
a method in order to assess compliance with effluent limits based on 
EPA and State water quality criteria for chlorine. Supporting 
performance data for the method can be found at Journal of the Water 
Pollution Control Federation, Vol. 51, pages 2636-2640 (1979), a copy 
of which is included in the docket for this proposal.

H. Replacement of Mercury Catalyst in Total Kjeldahl Nitrogen Methods

    Due to demonstrated toxic hazards of mercuric sulfate, and 
difficulty of disposal of laboratory wastes, EPA is proposing to 
replace this chemical with copper sulfate in the total Kjeldahl 
Nitrogen Methods. Copper sulfate exhibits significantly less toxicity 
than mercuric sulfate. The European community has already eliminated 
mercuric chloride from their total nitrogen methods in favor of less 
toxic catalysts.
    I. EPA is proposing to amend EPA Method 180.1--Turbidity by 
accepting the use of styrene divinylbenzene beads (AMCO-AEPA-1 
Standard) as a substitute for the presently used formazine standard, 
which is prepared from hydrazine sulfate. The AEPA-1 Standard is an 
alternate to formazine in the previously approved Standard Methods, 
Method 2130 B. This substitution will eliminate the need to use 
hydrazine sulfate, a known carcinogen.
    J. EPA is proposing to delete liquid-liquid extraction (LLE) 
methods, including EPA Methods 611 and 625 and Standard Methods Method 
6410 B, as approved procedures for 1,2-dichlorobenzene, 1,3-
dichlorobenzene, and 1,4-dichlorobenzene. While these compounds can be 
determined by these LLE methods, due to their volatility, significant 
losses can occur when using the prescribed sample collection procedures 
in the LLE methods resulting in low recovery of these compounds. These 
compounds are more properly analyzed by EPA Method 624 or Method 1625 
(an isotope-dilution method that compensates for any evaporation 
losses).
    K. EPA proposes to delete extraneous method citations, including 
those EPA methods that reference another source for method details and 
certain older EPA methods that are readily available from another 
source. Some measurement technologies are proposed for removal because 
they are no longer supported by the group that authored them or they 
use toxic reagents. EPA plans to provide an 18-month transition period 
after final rule to permit continued use of these methods following the 
practice of the drinking water program (see 59 FR 62456). These 
deletions include: colorimetric methods for cadmium, lead and zinc 
(dithizone), copper (neocuprione), nickel (heptoxime), nitrate-nitrite 
(automated hydrazine), potassium (cobaltinitrite), vanadium (gallic 
acid); AA furnace methods for gold, iridium, platinum, rhodium, 
ruthenium, titanium, and zinc; flame phometric methods for potassium 
and sodium; voltametry for cadmium and lead; titration (mercuric 
nitrate) for chloride; and the AA chelation-extraction for total 
chromium. Table IB of Part 136(a) would be further revised to reorder 
and clarify footnotes and method citations.

IV. Request for Comments

    The Agency requests general comments on its policy to remove or 
reject methods from this regulation on the basis of pollution 
prevention when comparable approved methods are available. Comments on 
the specific methods removed today are also solicited, as well as, 
comments on other pollution prevention changes that should be 
considered by the Agency. EPA considered the elimination of the Nessler 
method for Total Kjeldahl because the Nessler reagent contains 10% 
mercuric iodide. However, an assessment of the data submitted by 
participants in recent Water Pollution (WP) performance evaluation 
studies indicated that the Nessler method is broadly used and produces 
above-average data compared to the other approved methods. Further, the 
Nessler method may be necessary to this regulation because it is more 
sensitive than the other methods. The Agency requests comments on 
whether the Nessler methods should be removed from Part 136.

V. Regulatory Requirements

A. Executive Order 12866

    Under Executive Order 12866, EPA must determine whether a 
regulation is ``significant'' and, therefore subject to OMB review and 
the requirements of the Executive Order. EPA has determined that this 
regulation is not a ``significant regulatory action'' under the terms 
of Executive Order 12866 and is therefore not subject to OMB review. 
This rule will not result in an effect on the economy of $100 million 
or more, a significant increase in cost or prices, or any of the 
effects described in the Executive Order. This proposed rule simply 
specifies analytical techniques which may be used by laboratories in 
measuring concentrations of certain metals and, therefore, has no 
adverse economic impacts.

B. Regulatory Flexibility Act

    This proposed amendment is consistent with the objectives of the 
Regulatory Flexibility Act (5 U.S.C. 601 et seq.) because it will not 
have a significant economic impact on a substantial number of small 
entities. The procedures proposed in this rule give all laboratories 
the flexibility to use the new proposed procedures or already approved 
alternate procedures.

C. Paperwork Reduction Act

    This proposed rule contains no requests for information activities 
and, therefore, no information collection request (ICR) was submitted 
to the Office of Management and Budget (OMB) for review in compliance 
with the Paperwork Reduction Act, 44 U.S.C. 3501 et seq.

D. Unfunded Mandates

    Under Section 202 of the Unfunded Mandates Reform Act of 1995, 
signed into law on March 22, 1995, EPA must prepare a written statement 
to accompany rules where the estimated costs to State, local, or tribal 
governments, or to the private sector will be $100 million or more in 
any one year. Under Section 205, EPA must select the most cost-
effective and least burdensome alternative that achieves the objective 
of such a rule and that is consistent with statutory requirements. 
Section 203 requires EPA to establish a plan for informing and advising 
any small governments that may be significantly and uniquely affected 
by the rule.
    EPA estimates that the costs to State, local or tribal governments, 
or the private sector, from this proposed rule will be far less than 
$100 million. This proposed rule should have minimal impact, if any, on 
the existing regulatory burden imposed on NPDES permittees required to 
monitor for regulated pollutants because the proposed rule would merely 
make additional options 

[[Page 53992]]
available to the laboratory analyst conducting an existing approved 
test method. EPA has determined that an unfunded mandates statement 
therefore is unnecessary. Similarly, the methods proposed today do not 
establish any regulatory requirements that might significantly or 
uniquely affect small governments.

List of Subjects in 40 CFR Part 136

    Environmental protection, Incorporation by reference, Water 
pollution control.

    Dated: October 10, 1995.
Carol M. Browner,
Administrator.
    In consideration of the preceding, EPA proposes to amend part 136 
of title 40 of the Code of Federal Regulations as follows:

PART 136--[AMENDED]

    1. The authority citation for part 136 continues to read as 
follows:

    Authority: Secs. 301, 304(h), 307, and 501(a) Public Law 95-217, 
Stat. 1566, et seq. (33 U.S.C. 1251 et seq. (the Federal Water 
Pollution Control Act Amendments of 1972 as amended by the Clean 
Water Act of 1977).

    2. Section 136.3(a) is proposed to be amended by revising Table IB 
to read as follows:


Sec. 136.3  Identification of test procedures.

* * * * *

                                                                                                                

[[Page 53993]]
                                                                      Table IB.--List of Approved Inorganic Test Procedures                                                                     
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                               Reference (Method No. or Page)                                                   
                                                          --------------------------------------------------------------------------------------------------------------------------------------
    Parameter, Units and Method             EPA\1\                                                                                                                     AOAC-international\3\ and
                                                                Std. Methods 18th Ed.                     ASTM                                USGS\2\                            others         
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:                                                                                                                                                                     
    Electrometric or                 ....................  2310 B(4a)                       D1067-92                         ........................................  .........................
     phenolphthalein endpoint.                                                                                                                                                                  
2. Alkalinity, as CaCo3, mg/L:                                                                                                                                                                  
    Electrometric or colorimetric    ....................  2320 B                           D1067-92                         I-1030-85                                 973.43                   
     titration to pH 4.5, Manual,                                                                                                                                                               
     or.                                                                                                                                                                                        
    Automated......................           \15\310.215  ...............................  ...............................  I-2030-85                                 .........................
3. Aluminum--Total\4\, mg/L:                                                                                                                                                                    
    Digestion 5,6 followed by:                                                                                                                                                                  
        AA direct aspiration.......  ....................  3111 D                           ...............................  I-3051-85                                 .........................
        AA graphite furnace........                 200.9  3113 B                           ...............................  ........................................  .........................
        Inductively Coupled Plasma/                 200.7  3120 B                           ...............................  ........................................  .........................
         Atomic Emission                                                                                                                                                                        
         Spectrometry (ICP/AES).                                                                                                                                                                
        Inductively Coupled Plasma/                 200.8  ...............................  ...............................  ........................................  993.14                   
         Mass Spectrometry (ICP/MS).                                                                                                                                                            
        Direct Current Plasma        ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
         (DCP), or.                                                                                                                                                                             
        Colorimetric (Eriochrome     ....................   3500-Al D                       ...............................  ........................................  .........................
         cyanine R).                                                                                                                                                                            
4. Ammonia (as N), mg/L:                                                                                                                                                                        
    Manual, distillation (at pH                     350.1  4500-NH3 B                       ...............................  ........................................  973.49                   
     9.5)\7\, followed by:.                                                                                                                                                                     
        Nesslerization.............  ....................  4500-NH3 C                       D1426-93(A)                      I-3520-85...............................  973.49                   
        Titration..................  ....................  4500-NH3 E                       ...............................  ........................................  .........................
        Electrode..................  ....................  4500-NH3 F or G                  D1426-93(B)....................  ........................................  .........................
        Automated phenate, or......                 350.1  4500-NH3 H                       ...............................  I-4523-85                                 .........................
        Automated electrode........  ....................  ...............................  ...............................  ........................................  Note 17                  
5. Antimony-Total\4\, mg/L:                                                                                                                                                                     
  Digestion5 6 followed by:                                                                                                                                                                     
        AA direct aspiration.......  ....................   3111 B                          ...............................  ........................................  .........................
        AA graphite furnace........                 200.9  3113 B                           ...............................  ........................................  .........................
        ICP/AES, or................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
6. Arsenic-Total\4\, mg/L:                                                                                                                                                                      
    Digestion5 6 followed by:                                                                                                                                                                   
        AA gaseous hydride.........  ....................  3114 B 4.d                       D2972-93(B)                      I-3062-85                                 .........................
        AA graphite furnace........                 200.9  3113 B                           D2972-93(C)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        Colorimetric (SDDC)........  ....................  ...............................  D2972-93(A)                      I-3060-85                                 .........................
7. Barium--Total\4\ mg/L:                                                                                                                                                                       
    Digestion5 6 followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 D                           ...............................  I-3084-85                                 .........................
        AA graphite furnace........  ....................  3113 B                           D4382-91                         ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
8. Beryllium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................   3111 D                          D3645-93(A)                      I-3095-85                                 .........................
        AA graphite furnace........                 200.9  3113 B                           D3645-93(B)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP, or....................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
        Colorimetric (aluminon)....  ....................  3500-Be D                        ...............................  ........................................  .........................
9. Biochemical oxygen demand                                                                                                                                                                    
 (BOD5), mg/L:                                                                                                                                                                                  
    Dissolved Oxygen Depletion.....  ....................  5210 B                           ...............................  ........................................  973.44, p.17\18\         

[[Page 53994]]
                                                                                                                                                                                                
10. Boron\8\--Total, mg/L:                                                                                                                                                                      
    Colorimetric (curcumin)........  ....................  4500-B B                         ...............................  I-3112-85...............................  .........................
    ICP/AES, or....................                 200.7  3120 B                           ...............................  ........................................  .........................
    DCP............................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
11. Bromide, mg/L;                                                                                                                                                                              
    Titrimetric, or................  ....................  ...............................  D1246-82(88)(C)                  I-1125-85                                 p. S44\19\               
    Ion Chromatography.............                 300.0  4110 B                           D4327-91.......................  ........................................  993.30                   
12. Cadmium--Total\4\, mg/L:                                                                                                                                                                    
    Digestion\5\,\6\ followed by:                                                                                                                                                               
        AA direct aspiration.......  ....................  3111 B or C                      D3557-90(A or B)                 I-3135-85 or I-3136-85                    974.2 p. 37\18\          
        AA graphite furnace........                 200.9  3113 B                           D3557-90(D)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
13. Calcium--Total\4\, mg/L:                                                                                                                                                                    
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           D511-93(B)                       I-3152-85                                 .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        DCP, or....................  ....................  ...............................  ...............................  ........................................  Note 16                  
        Titrimetric (EDTA).........  ....................  3500-Ca D                        D511-93(A)                       ........................................  .........................
14. Carbonaceous biochemical oxygen  ....................  5210 B                           ...............................  ........................................  .........................
 demand (CBOD\5\), mg/L\9\.                                                                                                                                                                     
Dissolved Oxygen Depletion with                                                                                                                                                                 
 nitrification inhibitor                                                                                                                                                                        
15. Chemical oxygen demand (COD),                                                                                                                                                               
 mg/L:                                                                                                                                                                                          
    Titrimetric, or................             410.3\15\  5220 B                           D1252-88(A)                      I-3560-85, I-3562-85                      973.46, p. 17\18\        
    Spectrophotometric, manual or                   410.4  5220 D                           D1252-88(B)                      I-3561-85                                 Notes 20, 21             
     automated.                                                                                                                                                                                 
16. Chloride, mg/L:                                                                                                                                                                             
    Titrimetric (silver nitrate)...                        4500-Cl B                        D512-89(B)                       I-1183-85                                 .........................
    Colorimetric, Manual, or.......  ....................  ...............................  ...............................  I-1187-85...............................  .........................
        Automated (Ferricyanide),    ....................  4500-Cl-E                        ...............................  I-2187-85...............................  .........................
         or.                                                                                                                                                                                    
    Ion Chromatography.............                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
17. Chlorine--Total residual, mg/L:                                                                                                                                                             
    Titrimetric: Amperometric        ....................  4500-Cl D or E                   D1253-86(92)                     ........................................  .........................
     direct.                                                                                                                                                                                    
        Iodometric direct..........  ....................  4500-Cl B                        ...............................  ........................................  .........................
        Back titration either end-                         4500-Cl C                        ...............................  ........................................  .........................
         point\10\.                                                                                                                                                                             
        DPD-FAS....................  ....................  4500-Cl F                        ...............................  ........................................  .........................
    Spectrophotometric (DPD), or...  ....................  4500-Cl G                        ...............................  ........................................  .........................
    Electrode......................  ....................  ...............................  ...............................  ........................................  Note 22                  
18. Chromium VI dissolved, mg/L:                                                                                                                                                                
    0.45 micron filtration followed                                                                                                                                                             
     by:                                                                                                                                                                                        
        AA chelation-extraction....  ....................  3111 C                           ...............................  I-1232-85                                 .........................
        Ion Chromatography, or.....                 218.6  3500-Cr E\23\                    D5257-93                         ........................................  993.23                   
        Colorimetric                 ....................  3500-Cr D                        D1687-92(A)                      I-1230-85                                 .........................
         (Diphenylcarbazide).                                                                                                                                                                   
19. Chromium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion\5\,\66\ followed by:                                                                                                                                                              
        AA direct aspiration.......  ....................                                   D1687-92(B)                      I-3236-85                                 974.27                   
        AA graphite furnace........                 200.9  3113 B                           D1687-92(C)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B.........................  ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
        Colorimetric                 ....................  3500-Cr D                        ...............................  ........................................  .........................
         (Diphenylcarbazide).                                                                                                                                                                   
20. Cobalt--Total\4\, mg/L:                                                                                                                                                                     

[[Page 53995]]
                                                                                                                                                                                                
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B or C                      D3558-90(A or B)                 I-3239-85                                 p.37\18\                 
        AA graphite furnace........                 200.9  3113 B                           D3558-90(C)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
21. Color, platinum cobalt units or                                                                                                                                                             
 dominant wavelength, hue,                                                                                                                                                                      
 luminance purity:                                                                                                                                                                              
    Colorimetric (ADMI)............  ....................  2120 E                           ...............................  ........................................  Note 24                  
    Colorimetric (Platinum cobalt),  ....................   2120B                           ...............................  I-1250-85...............................  .........................
     or.                                                                                                                                                                                        
    Spectrophotometric.............  ....................  2120 C                           ...............................  ........................................  .........................
22. Copper--Total\4\, mg/L:                                                                                                                                                                     
    Digestion5,6 followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................   3111 B or C                     D1688-90(A or B)                 I-3270-85 or I-3271-85                    974.27p.37\18\           
        AA graphite furnace........                 200.9  3113 B                           D1688-90(C)                                                                                         
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP, or....................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
        Colorimetric                 ....................  ...............................  ...............................  ........................................  Note 25                  
         (Bicinchoninate).                                                                                                                                                                      
23. Cyanide--Total, mg/L:                                                                                                                                                                       
    Manual distillation\11\ with                    335.4  4500-CN C                        D2036-91(A)                      ........................................  .........................
     MgCl2 followed by:                                                                                                                                                                         
        Titrimetric................  ....................  4500-CN D                        ...............................  ........................................  p.22\19\                 
        Spectrophotometric, manual   ....................  4500-CN E                        D2036-91(A)                      I-3300-85                                 .........................
         or.                                                                                                                                                                                    
        Spectrophotometric,                         335.4  ...............................  ...............................  ........................................  .........................
         automated.                                                                                                                                                                             
24. Cyanide amenable to                                                                                                                                                                         
 chlorination, mg/L:                                                                                                                                                                            
    Manual distillation with MgCl2,  ....................  4500-CN G                        D2036-91(B)....................  ........................................  .........................
     followed by titrimetric or                                                                                                                                                                 
     spectrophotometric.                                                                                                                                                                        
25. Fluoride--Total, mg/L:                                                                                                                                                                      
    Manual distillation\7\,          ....................  4500-F B                         ...............................  ........................................  .........................
     followed by:                                                                                                                                                                               
        Electrode, Manual..........  ....................  4500-F C                         D1179-93(B)....................  ........................................  .........................
        Electrode, Automated.......  ....................  ...............................  ...............................  I-4327-85                                 .........................
        Colorimetric (SPADNS)......  ....................  4500-F D                         D1179-93(A)                      ........................................  .........................
        Colorimetric (Auto           ....................  4500-F-E                         ...............................  ........................................  .........................
         complexone), or.                                                                                                                                                                       
        Ion Chromatography.........                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
26. Gold--Total\4\, mg/L:                                                                                                                                                                       
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration, or...  ....................  3111 B                           ...............................  ........................................  .........................
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
27. Hardness--Total, as CaCO\3\, mg/                                                                                                                                                            
 L:                                                                                                                                                                                             
    Automated colorimetric.........             130.1\15\  ...............................  ...............................  ........................................  .........................
    Titrimetric (EDTA), or.........  ....................  2340 B or C                      D1126-86(92)                     I-1338-85                                 973.52B                  
    Ca plus Mg as their carbonates,                                                                                                                                                             
     by ICP/AES, AA direct                                                                                                                                                                      
     aspiration, or DCP.                                                                                                                                                                        
     (Parameters 13 and 33).                                                                                                                                                                    
28. Hydrogen ion (pH), pH units:                                                                                                                                                                
    Electrometric measurement, or..  ....................  4500-H+ B                        D1293-84(90) (A or B)            I-1586-85                                 973.41                   
    Automated electrode............             150.2\15\  ...............................  ...............................  ........................................  Note 26                  
29. Iridium--Total\4\, mg/L:                                                                                                                                                                    
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           ...............................  ........................................  .........................
30. Iron--Total\4\, mg/L:                                                                                                                                                                       
     Digestion5,6 followed by:                                                                                                                                                                  
        AA direct aspiration.......  ....................  3111 B D                         D1068-90(A or B)                 I-3381-85                                 974.27                   
        AA graphite furnace........                 200.9  3113 B                           D1068-90(C)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        DCP, or....................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
        Colorimetric                 ....................  ...............................  ...............................  ........................................  Note 27                  
         (Phenanthroline).                                                                                                                                                                      
31. Kjeldahl nitrogen--Total, (as                                                                                                                                                               
 N), mg/L:                                                                                                                                                                                      
    Digestion\12\ and distillation.                                                                                                                                                             

[[Page 53996]]
                                                                                                                                                                                                
    followed by:                     ....................  4500-Norg B or C...............  D3590-89(A)                      ........................................  .........................
        Titration..................  ....................  4500-NH3 E                       D3590-89(A)                      ........................................  973.48                   
        Nesslerization, or.........  ....................  4500-NH3 C                       D3590-89(A)                      ........................................  .........................
        Electrode..................  ....................  4500-NH3 F or G                  ...............................  ........................................                           
    Colorimetric (Automated                    l351.1\15\  ...............................  ...............................  ........................................  .........................
     phenate)\12\.                                                                                                                                                                              
    Semi-automated block                            351.2  ...............................  D3590-89(B)                      ........................................  .........................
     digestor\12\ colorimetric, or.                                                                                                                                                             
    Manual or block digestor\12\     ....................  ...............................  D3590-89(A)                      ........................................  .........................
     potentiometric.                                                                                                                                                                            
    Block digestor, followed by:     ....................  ...............................  ...............................  ........................................  Note 28                  
     Auto distillation and                                                                                                                                                                      
     Titration, or                                                                                                                                                                              
    Nesslerization or..............  ....................  ...............................  ...............................  ........................................  Note 29                  
    Flow injection gas diffusion...  ....................  ...............................  ...............................  ........................................  Note 30                  
32. Lead--Total\4\, mg/L:                                                                                                                                                                       
    Digestion\5\ \6\ followed by:                                                                                                                                                               
        AA direct aspiration.......  ....................  3111 B or C                      D3559-90(A or B)                 I-3399-85                                 974.27                   
        AA graphite furnace........                 200.9  3113 B                           D3559-90(D)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
33. Magnesium--Total\4\, mg/L:                                                                                                                                                                  
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           D511-93(B)                       I-3447-85                                 974.27                   
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
        Gravimetric................  ....................  3500-Mg D                        ...............................  ........................................  .........................
34. Manganese--Total\4\, mg/L:                                                                                                                                                                  
    Digestion5,6 followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           D858-90(A or B)                  I-3454-85                                 974.27                   
        AA graphite furnace........                 200.9  3113 B                           D858-90(C)                       ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
        Colorimetric (Persulfate),   ....................  ...............................  ...............................  ........................................  920.203                  
         or.                                                                                                                                                                                    
        Colorimetric (Periodate)...  ....................  ...............................  ...............................  ........................................  Note 31                  
35. Mercury--Total\4\, mg/L                                                                                                                                                                     
    Cold vapor, manual, or.........                 245.1  3112 B                           D3223-91                         I-3462-85                                 977.22                   
    Cold vapor, automated..........                 245.2  ...............................  ...............................  ........................................  .........................
36. Molybdenum--Total\4\, mg/L:                                                                                                                                                                 
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 D                           ...............................  I-3490-85                                 .........................
        AA graphite furnace........  ....................  3113 B                           ...............................  ........................................  .........................
        ICP/AES....................                 200.7  3120B                            ...............................  ........................................  .........................
        ICP/MS, OR.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
37. Nickel--Total \4\, mg/L:                                                                                                                                                                    
    Digestion\5\ \6\ followed by:                                                                                                                                                               
        AA direct aspiration.......  ....................  3111 B or C                      D1886-90(A or B)                 I-3499-85                                 .........................
        AA graphite furnace........                 200.9  3113 B                           D1886-90(C)                      ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  D4190-82(88)                     ........................................  Note 16                  
38. Nitrate (as N), mg/L:                                                                                                                                                                       
    Colorimetric (Brucine sulfate).             \15\352.1  ...............................  ...............................  ........................................  973.50, p.28\18\         

[[Page 53997]]
                                                                                                                                                                                                
    Ion Chromatography, or.........                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
    Nitrate-nitrite N minus Nitrite                                                                                                                                                             
     N (See parameters 39 and 40)                                                                                                                                                               
39. Nitrate-nitrite (sum as N), mg/                                                                                                                                                             
 L:                                                                                                                                                                                             
    Cadmium reduction, Manual......  ....................  4500-NO3 E                       D3867-90(B)                      ........................................  .........................
    Cadmium reduction, Automated,                   353.2  4500-NO3 F                       D3867-90(A)                      I-4545-85                                 .........................
     or.                                                                                                                                                                                        
    Ion Chromatography.............                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
40. Nitrite (as N), mg/L:                                                                                                                                                                       
    Spectrophotometric, Manual, or.  ....................  4500-NO2 B                       ...............................  ........................................  Note 32                  
        Automated (Diazotization)..  ....................  ...............................  ...............................  I-4540-85                                 .........................
    Cadmium reduction, Manual......  ....................  4500-NO3 E.....................  D3867-90(B)                      ........................................  .........................
    Cadmium reduction, Automated,                   353.2  4500-NO3 F                       D3867-90(A)                      I-4545-85                                 .........................
     or.                                                                                                                                                                                        
    Ion Chromatography.............                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
41. Oil and grease--Total                                                                                                                                                                       
 recoverable, mg/L:                                                                                                                                                                             
    Gravimetric (extraction).......                 413.1  5520-B\33\                       ...............................  ........................................  .........................
42. Organic carbon--Total (TOC), mg/                                                                                                                                                            
 L:                                                                                                                                                                                             
    Combustion or oxidation........  ....................  5310-B,C or D                    D2579-93(A or B)                 ........................................  973.47, p.14\35\         
43. Organic nitrogen (as N), mg/L:                                                                                                                                                              
    Total Kjeldahl N (Parameter 31)                                                                                                                                                             
     minus ammonia N (Parameter 4)                                                                                                                                                              
44. Orthophosphate (as P), mg/L:                                                                                                                                                                
    Ascorbic acid method:                                                                                                                                                                       
        Automated, or..............                 365.1  4500-P F                         ...............................  I-4601-85                                 973.56                   
        Manual single reagent......  ....................  4500-P E                         D515-88(A)                       ........................................  973.55                   
        Manual two reagent, or.....             365.3\15\  ...............................  ...............................  ........................................  .........................
    Ion Chromatography.............                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
45. Osmium--Total,\4\ mg/L:                                                                                                                                                                     
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration, or...  ....................  3111 D                           ...............................  ........................................  .........................
        AA graphite furnace........  ....................  ...............................  ...............................  ........................................  .........................
46. Oxygen dissolved, mg/L:                                                                                                                                                                     
    Winkler (Azide modification),    ....................  4500-O C                         D888-92(A)                       ........................................  973.45B                  
     or.                                                                                                                                                                                        
    Electrode......................  ....................  4500-O G                         D888-92(B)                       ........................................  .........................
47. Palladium--Total,\4\ mg/L:                                                                                                                                                                  
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration,        ....................  3111 B                           ...............................  ........................................  p.S27\19\                
        AA graphite furnace, or....  ....................  ...............................  ...............................  p.S28\19\...............................                           
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
48. (Reserved)                                                                                                                                                                                  
49. Phenols, mg/L:                                                                                                                                                                              
    Manual distillation,\13\                                                                                                                                                                    
     followed by                                                                                                                                                                                
        Colorimetric (4AAP) manual,             \15\420.1  ...............................  ...............................  ........................................  Note 35                  
         or.                                                                                                                                                                                    
        Colorimetric (4AAP)                         420.4  ...............................  ...............................  ........................................  .........................
         Automated.                                                                                                                                                                             
50. Phosphorus (elemental), mg/L     ....................  ...............................  ...............................  ........................................  Note 36                  
 Gas-liquid chromatography.                                                                                                                                                                     
51. Phosphorus--Total, mg/L:                                                                                                                                                                    
    Persulfate digestion followed    ....................  4500-P B,5                       ...............................  ........................................  973.55                   
     by:.                                                                                                                                                                                       
        Ascorbic acid reduction,                365.3\15\  4500-P E                         D515-88(A)                       ........................................  .........................
         Manual, or.                                                                                                                                                                            
        Automated..................                 365.1  4500-P F                         ...............................  I-4600-85...............................  973.56                   
    Semi-automated block digestor..  ....................  ...............................  D515-88(B)                       ........................................  .........................
52. Platinum--Total\4\, mg/L;                                                                                                                                                                   
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration, or...  ....................  3111 B                           ...............................  ........................................  .........................
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
53. Potassium--Total\4\, mg/L;                                                                                                                                                                  
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration, or...  ....................  3111 B                           ...............................  I-3630-85                                 973.53                   
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
54. Residue--Total, mg/L:                                                                                                                                                                       
    Gravimetric, 103-105 deg.......  ....................  2540 B                           ...............................  I-3750-85                                 .........................
55. Residue--filterable, mg/L;                                                                                                                                                                  
    Gravimetric, 180 deg...........  ....................  2540 C                           ...............................  I-1750-85                                 .........................

[[Page 53998]]
                                                                                                                                                                                                
56. Residue--nonfilterable (TSS),                                                                                                                                                               
 mg/L:                                                                                                                                                                                          
    Gravimetric, 103-105 deg. post   ....................  2540 D                           ...............................  I-3765-85                                 .........................
     washing of residue.                                                                                                                                                                        
57. Residue--settleable, mg/L:                                                                                                                                                                  
    Volumetric (Imhoff cone), or     ....................  2540 F                           ...............................  ........................................  .........................
     Gravimetric.                                                                                                                                                                               
58. Residue--Volatile, mg/L:                                                                                                                                                                    
    Gravimetric, 550 deg. C........             160.4\15\  ...............................  ...............................  I-3753-85                                 .........................
59. Rhodium--Total\4\, mg/L:                                                                                                                                                                    
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           ...............................  ........................................  .........................
60. Ruthenium--Total\4\, mg/L:                                                                                                                                                                  
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           ...............................  ........................................  .........................
61. Selenium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion5,6 followed by:                                                                                                                                                                   
        AA graphite furnace........                 200.9  3113 B                           D3859-93(B)                      ........................................  .........................
        AA gaseous hydride.........  ....................  3114 B                           3859-93(A)                       I-3667-85                                 .........................
        ICP/AES, or................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
62. Silica\8\ Dissolved, mg/L:                                                                                                                                                                  
    0.45 micron filtration followed                                                                                                                                                             
     by:                                                                                                                                                                                        
        Colorimetric , Manual, or..  ....................  4500-Si D                        D859-88                          I-1700-85                                 .........................
        Automated                    ....................  ...............................  ...............................  I-2700-85                                 .........................
         (Molybdosilicate), or.                                                                                                                                                                 
        ICP........................                 200.7  3120 B                           ...............................  ........................................  .........................
63. Silver--Total\4\, mg/L:                                                                                                                                                                     
    Digestion5,14 followed by:                                                                                                                                                                  
        AA direct aspiration.......  ....................  3111 B or C                      ...............................  ........................................  974.27, p.37\18\         
        AA graphite furnace........                 200.9  3113 B                           ...............................  ........................................  .........................
        ICP/AES....................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
64. Sodium--Total\4\, mg/L:                                                                                                                                                                     
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           ...............................  I-3735-85                                 973.54                   
        ICP/AES, or................                 200.7  3120 B                           ...............................  ........................................  .........................
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
65. Specific conductance, micromhos/                                                                                                                                                            
 cm at 25 deg.C:                                                                                                                                                                                
    Wheatstone bridge..............  ....................  2510 B                           D1125-91(A)                      I-1780-85                                 973.40                   
66. Sulfate (as SO4), mg/L:                                                                                                                                                                     
    Colorimetric, Automated (Barium             375.1\15\  ...............................  ...............................  ........................................  .........................
     chloranilate).                                                                                                                                                                             
    Gravimetric....................  ....................  4500-SO4-2 C or D                ...............................  ........................................  925.54                   
    Turbidimetric, or..............  ....................  4500-SO4-2 E                     D516-90........................  ........................................  .........................
    Ion Chromatography.............                 300.0  4110 B                           D4327-91                         ........................................  993.30                   
67. Sulfide (as S), mg/L:                                                                                                                                                                       
    Titrimetric (iodine), or.......  ....................  4500-S-2 E                       ...............................  I-3840-85                                 .........................
    Colorimetric (methylene blue)..  ....................  4500-S-2 D                       ...............................  ........................................  .........................
68. Sulfite (as SO3), mg/L:                                                                                                                                                                     
    Titrimetric (iodine-iodate)....  ....................  4500-SO3-2 B                     ...............................  ........................................  .........................
69. Surfactants, mg/L:                                                                                                                                                                          
    Colorimetric (methylene blue)..  ....................  5540 C                           D2330-88.......................  ........................................  .........................
70. Temperature,  deg.C:                                                                                                                                                                        

[[Page 53999]]
                                                                                                                                                                                                
    Thermometric...................  ....................  2550 B                           ...............................  ........................................  Note 37                  
71. Thallium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 B                           ...............................  ........................................  .........................
        AA graphite furnace........                 200.9  ...............................  ...............................  ........................................  .........................
        ICP/AES, or................                 200.7  3120 B                           ...............................  ........................................  .........................
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
72. Tin--Total\4\, mg/L:                                                                                                                                                                        
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration,......  ....................  3111 B                                                                                                                               
        AA graphite furnace, or....                 200.9  3113 B.........................                                                                                                      
        ICP/AES....................                 200.7  ...............................                                                                                                      
73. Titanium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 D                                                                                                                               
        ICP/AES, or................                 200.7                                                                                                                                       
        DCP........................  ....................  ...............................  ...............................  ........................................  Note 16                  
74. Turbidity, NTU:                                                                                                                                                                             
    Nephelometric..................                 180.1  2130 B                           D1889-88(A)                      I-3860-85                                                          
75. Vanadium--Total\4\, mg/L:                                                                                                                                                                   
    Digestion\5\ followed by:                                                                                                                                                                   
        AA direct aspiration.......  ....................  3111 D                                                                                                                               
        AA graphite furnace........  ....................  ...............................  D3373-93                                                                                            
        ICP/AES....................                 200.7  3120 B                                                                                                                               
        ICP/MS, or.................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP........................  ....................  ...............................  ...............................  D4190-82(88)............................  Note 16                  
76. Zinc--Total\4\, mg/L:                                                                                                                                                                       
    Digestion\5\,\6\ followed by:                                                                                                                                                               
        AA direct aspiration.......  ....................  3111 (B or C)                    D1691-90 (A or B)                I-3900-85                                 974.27, p. 37\18\        
        ICP/AES....................                 200.7  3120 B                                                                                                                               
        ICP/MS.....................                 200.8  ...............................  ...............................  ........................................  993.14                   
        DCP, or....................  ....................  ...............................  D4190-82(88)...................  ........................................  Note 16                  
        Colorimetric (zincon)......  ....................  3500-Zn F                        ...............................  ........................................  Note 38                  
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB--Notes                                                                                                                                                                                 
                                                                                                                                                                                                
 \1\``Methods for the Determination of Metals in Environmental Samples'', Supplement I, EMSL-CI, EPA/600/R-94/111, May 1994; and ``Methods for the Determination of Inorganic Substances in     
  Environmental Samples'', EMSL-CI, EPA/600/R-93/100, August, 1993.                                                                                                                             
\2\Fishman, M. J., et al., ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments'', U.S. Department of the Interior, Techniques of Water--Resource Investigations of the
  U.S. Geological Survey (USGS), Denver, CO, Revised 1989.                                                                                                                                      
\3\``Official Methods of Analysis of the Association of Official Analytical Chemists'', methods manual, 16th ed (1995).                                                                         
\4\For the determination of total metals the sample is not filtered before processing and a digestion procedure is required a) to solubilize analytes in the suspended material and b) to render
  the analyte available for analysis when colorimetric methods are used.                                                                                                                        
\5\For non-platform graphite furnace atomic absorption determinations a digestion using nitric acid is reguired prior to analysis. The procedure used should subject the sample to gentle, acid 
  refluxing and at no time should the sample be taken to dryness. For direct aspiration flame atomic absorption determinations (FLAA) a combination acid (nitric and hydrochloric acids)        
  digestion is preferred prior to analysis. Such a digestion is described as Method 200.2 in Supplement I of ``Methods for the Determination of Metals in Environmental Samples'' EPA-600/R-94/ 
  111 May, 1994. However, when using the gaseous hydride technique or for the determination of certain elements such as antimony, arsenic, selenium, silver, and tin by non-EPA graphite furnace
  atomic absorption methods, mercury by cold vapor atomic absorption, the noble metals and titanium by FLAA, a specific or modified sample digestion procedure may be required and in all cases 
  the referenced method write-up should be consulted for specific instruction and/or cautions. For analyses using inductively coupled plasma-atomic emission spectrometry (ICP-AES), the direct 
  current plasma (DCP) technique or the EPA spectrochemical techniques (platform furnace AA, ICP-AES, and ICP-MS) the appropriate sample digestion procedure to be used is included in the      
  referenced Standard Methods, ASTM, Fisons, or EPA methods, respectively.                                                                                                                      
\6\The digestion procedure ``Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals'', CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200, April 16, 1992, is  
  acceptable for use with any AA direct aspiration, ICP/AES, or DCP measurement system listed for this parameter. Available from the CEM Corporation.                                           
\7\Manual distillation is not required if comparability data on representative effluent samples are on company file to show that this preliminary distillation step is not necessary; however,  
  manual distillation will be required to resolve any controversies.                                                                                                                            
\8\When determining boron and silica, only plastic, PFTE, or quartz labware may be used from start until completion of the analysis.                                                            
\9\Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test which measures ``total BOD''. The addition of the nitrification inhibitor is not a        
  procedural option, but must be included to report the CBOD5 parameter. A discharger whose permit requires reporting the traditional BOD5 may not use a nitrification inhibitor in the         
  procedure for reporting the results. Only when a discharger's permit specifically states CBOD5 is required can the permittee report data using the nitrification inhibitor.                   
\10\The back titration method will be used to resolve controversy.                                                                                                                              
\11\When using EPA digestion procedure, must use EPA determinative procedure. When using Standard Methods digestion procedure, must use Standard Methods determinative procedure.               
\12\Copper sulfate or other mercury-free catalyst shown to be effective must be used in place of mercuric sulfate in the digestion step.                                                        

[[Page 54000]]
                                                                                                                                                                                                
\13\Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.                                                                                              
\14\The digestion procedures in the approved Standard Methods direct aspiration flame atomic absorption and inductively coupled plasma-atomic emission spectrometry methods are useful for the  
  analysis of silver up to concentrations of 1 mg/l. However, where silver concentrations > 1 mg/L exist as an inorganic halide the referenced methods sample preparation procedures are        
  inadequate. For sample preparation in these situations a well-mixed representative 20 ml sample aliquot should be diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH prior to     
  analysis by direct aspiration flame atomic absorption. Calibration standards should be prepared in the same manner. The approved EPA methods are useful for the analysis of silver up to      
  concentrations of 0.1 mg/L.                                                                                                                                                                   
\15\``Methods for Chemical Analysis of Water and Wastes'', U.S. Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-CI), Cincinnati, OH, EPA-600/4-79-
  020, Revised March 1983 and 1979 where applicable.                                                                                                                                            
\16\``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AE50029'', 1986--Revised 1991, Fison Instruments, Inc., 32     
  Commerce Center, Cherry Hill Drive, Danvers, MA 01923.                                                                                                                                        
\17\Ammonia, Automated Electrode Method, Industrial Method Number 379-75 WE, dated February 19, 1976, Bran & Luebbe (Technicon) Auto Analyzer II, Bran & Luebbe Analyzing Technologies, Inc.,   
  Elmsford, NY 10523.                                                                                                                                                                           
\18\American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 1430 Broadway, New York, NY 10018.                                                      
\19\``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of Standard Methods for the Examination of     
  Water and Wastewater (1981).                                                                                                                                                                  
\20\OIC Chemical Oxygen Demand Method Oceanography International Corporation, 512 West Loop, P.O. Box 2980, College Station, TX 77840.                                                          
\21\Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.                                                        
\22\Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA 02138.                                     
\23\``Standard Method for the Examination of Water and Wastewater--Supplement to the 18th Edition'', 1994.                                                                                      
\24\National Council of the Paper Industry for Air and Stream Improvement (Inc.), Technical Bulletin 253, December 1971.                                                                        
\25\Copper, Biocinchoninate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.                                                
\26\Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Technicon AutoAnalyzer II, Technicon Industrial Systems, Tarrytown, NY 10591.                
\27\Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O.Box 389, Loveland, CO 80537.                                                                                
\28\Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, Perstop Analytical.                                               
\29\Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection), revised 12/22/94, Perstop Analytical.                                              
\30\Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion), revised 12/22/94, Perstop Analytical.                                                             
\31\Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company, Loveland, CO 80537.                           
\32\Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.                                                                                                    
\33\Only the trichlorotrifluoroethane extraction solvent option is approved.                                                                                                                    
\34\Wershaw, R.L., et al, ``Methods for Analysis of Organic Substances in Water'', Techniques of Water-Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A3 (1972 Revised  
  1987), p.14.                                                                                                                                                                                  
\35\The approved method is cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition. The colorimetric reaction is conducted at a pH of 10.00.2. The      
  approved methods are given on pp 576-81 of the 14th Edition: Method 510A for distillation, Method 510B for the manual colorimetric procedure, or Method 510C for the manual spectrophotometric
  procedure.                                                                                                                                                                                    
\36\R. F. Addison and R. G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography'', Journal of Chromatography, vol. 47, No. 3, pp. 421-426, 1970.                
\37\Stevens, H. H., Ficke, J. F., and Smoot, G. F., ``Water Temperature--Influential Factors, Field Measurement and Data Presentation'', U.S. Geological Survey, Techniques of Water Resources  
  Investigations, Book 1, Chapter D1, 1975.                                                                                                                                                     
\38\Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.                                                  



[[Page 54001]]

    3. Section 136.3(a) is proposed to be amended by revising entries 
35-37 of Table IC to read:


136.3  Identification of Test Procedures.

* * * * *

                                                         Table 1C.--List of Approved Test Procedures For Non-Pesticide Organic Compounds                                                        
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                            EPA Method Number2,7                                                                                                                
            Parameter\1\            -------------------------------------------------------------------     Standard methods 18th Ed.                ASTM                        Other          
                                         GC                GC/MS                       HPLC                                                                                                     
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
                                                                                                                                                                                                
                                       *                  *                  *                  *                  *                  *                  *                                      
35. 1,2-Dichlorobenzene............    601,602  624, 1625.................  --........................  6220 B, 6230 B..................                                                        
36. 1,3-Dichlorobenzene............    601,602  624, 1625.................  --........................  6220 B, 6230 B..................                                                        
37. 1,4-Dichlorobenzene............    601,602  624, 1625.................  --........................  6220 B, 6230 B..................                                                        
                                                                                                                                                                                                
                                       *                  *                  *                  *                  *                  *                  *                                      
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1C Notes                                                                                                                                                                                  
\1\All parameters are expressed in micrograms per liter (g/L).                                                                                                                         
\2\The full text of Methods 601-613, 624, 625, 1624, and 1625, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The standardized test         
  procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B, ``Definition and Procedure for the Determination of the Method Detection 
  Limit'' of this Part 136.                                                                                                                                                                     
                                                                                                                                                                                                
*                  *                  *                  *                  *                  *                  *                                                                             
\7\Each Analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-603, 624, 625, 1624, and 1625 (See Appendix A of   
  this Part 136) 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 and  
  625 and 100% for Methods 1624 and 1625) of all samples to monitor and evaluate laboratory data quality in accordance with sections 8.3 and 8.4 of these Methods. When the recovery of any     
  parameter falls outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory compliance. Note:   
  These warning limits are promulgated as an ``interim final action with a request for comments.''                                                                                              
                                                                                                                                                                                                
*                  *                  *                  *                  *                  *                  *                                                                             

    4. Section 136.3(b) is proposed to be amended by revising 
references 1 through 38 and adding references 39 and 40 to read as 
follows:


Sec. 136.3  Identification of test procedures.

* * * * *
    (b) * * *
References, Sources, Costs, and Table Citations
    (1) The full text of Methods 601-613, 624, 625, 1624, and 1625 are 
printed in appendix A of this part 136. The full text for determining 
the method detection limit when using the test procedures is given in 
appendix B of this part 136. Table IC, Note 7; and Table ID, Note 2.
    (2) ``Microbiological Methods for Monitoring the Environment, Water 
and Wastes,'' U.S. Environmental Protection Agency, EPA-600/8-78-017, 
1978. Available from: ORD Publications, CERI, U.S. Environmental 
Protection Agency, Cincinnati, Ohio 45268. Table IA. Note 2.
    (3) ``Methods for Chemical Analysis of Water and Wastes,'' U.S. 
Environmental Protection Agency, EPA 600/4-79-020, March 1979, or 
``Methods for Chemical Analysis of Water and Wastes, U.S. Environmental 
Protection Agency, EPA-600/4-79-020, Revised March 1983. Available 
from: ORD Publications, CERI, U.S. Environmental Protection Agency, 
Cincinnati, Ohio 45268. Table IB, Note 15.
    (4) ``Methods for Benzidine, Chlorinated Organic Compounds, 
Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. 
Environmental Protection Agency, 1978. Available from: ORD 
Publications, CERI, U.S. Environmental Protection Agency, Cincinnati, 
Ohio 45268, Table IC, Note 3; Table D, Note 3.
    (5) ``Prescribed Procedures for Measurement of Radioactivity in 
Drinking Water,'' U.S. Environmental Protection Agency, EPA-600/4-80-
032, 1980. Available from: ORD Publications, CERI, U.S. Environmental 
Protection Agency, Cincinnati, Ohio 45268, Table IE, Note 1.
    (6) ``Standard Methods for the Examination of Water and 
Wastewater'', Joint Editorial Board, American Public Health 
Association, American Water Works Association, and Water Environment 
Federation, 18th Edition, 1992. Available from: American Public Health 
Association, 1015 Fifteenth Street, NW., Washington, DC 20005, Cost 
$160.00. Table IA, IB, IC, ID and IE.
    (7) (Reserved)
    (8) Ibid, 14th Edition, 1975. Table IB, Note 35.
    (9) ``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. 
Available from: American Public Health Association, 1015 Fifteenth 
Street NW., Washington, DC 20036. Cost available from publisher. Table 
IB, Note 19; Table IC, Note 6; Table ID, Note 6.
     (10) ``Annual Book of Standards--Water and Environmental 
Technology'', Section 11, Parts 11.01 Water (I) and 11.02 Water (II), 
American Society for Testing and Materials, 1994. 1916 Race Street, 
Philadelphia, PA 19103. Cost available from publisher. Tables IB, IC, 
ID, and IE.
    (11) ``Methods for Collection and Analysis of Aquatic Biological 
and Microbiological Samples,'' edited by Britton, L.J. and P.E. 
Greason, Techniques of Water Resources Investigations, of the U.S. 
Geological Survey, Book 5, Chapter A4 (1989). Available from: U.S. 
Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. 
Cost: $9.25 (subject to change). Table IA.
    (12) ``Methods for Determination of Inorganic Substances in Water 
and Fluvial Sediments,'' by M.J. Fishman and Linda C. Friedman, 
Techniques of Water-Resources Investigations of the U.S. Geological 
Survey, Book 5 Chapter A1 (1989). Available from: U.S. Geological 
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost 
$108.75 (subject to change). Table IB, Note 2.
    (13) (Reserved)
    (14) ``Methods for the Determination of Organic Substances in Water 
and Fluvial Sediments, Wershaw, R.L., et al., Techniques of Water-
Resources 

[[Page 54002]]
Investigations of the U.S. Geological Survey, Book 5, Chapter A3 
(1987). Available from: U.S. Geological Survey, Denver Federal Center, 
Box 25425. Cost: $0.90 (subject to change). Table IB, Note 34, Table 
ID, Note 4.
    (15) ``Water Temperature-Influential Factors, Field Measurement and 
Data Presentation,'' by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot, 
Techniques of Water Resources Investigations of the U.S. Geological 
Survey, Book 1, Chapter D1, 1975. Available from: U.S. Geological 
Survey, Denver Federal Center, Box 25425, Denver, CO 80225, Cost: $1.60 
(subject to change). Table IB, Note 37.
    (16) ``Selected Methods of the U.S. Geological Survey of Analysis 
of Wastewaters, by M.J. Fishman and Eugene Brown; U.S. Geological 
Survey Open File Report 76-77 (1976). Available from: U.S. Geological 
Survey, Branch of Distribution, 1200 South Eads Street, Arlington, VA 
22202. Cost: $13.50 (subject to change). Table IE, Note 2.
    (17) ``Official Methods of Analysis of AOAC-International'', 16th 
Edition (1995). Price: $359.00. Available from: AOAC-International, 
1970 Chain Bridge Rd., Dept. 0742, McLean, VA 22109-0742. Table IB, 
Note 3.
    (18) ``American National Standard on Photographic Processing 
Effluents,'' April 2, 1975. Available from: American National Standards 
Institute, 1430 Broadway, New York, New York 10018. Table IB, Note 18.
    (19) ``An Investigation of Improved Procedures for Measurement of 
Mill Effluent and Receiving Water Color, NCASI Technical Bulletin No. 
253, December 1971. Available from: National Council of the Paper 
Industry for Air and Stream Improvements, Inc., 260 Madison Avenue, New 
York, NY 10016. Cost available from publisher. Table IB, Note 24.
    (20) Ammonia, Automated Electrode Method, Industrial Method Number 
379-75WE, dated February 19, 1976. Technicon Auto Analyzer II. Method 
and price available from Technicon Industrial Systems, Tarrytown, New 
York 10591. Table IB, Note 17.
    (21) Chemical Oxygen Demand, Method 8000, Hach Handbook of Water 
Analysis, 1979. Method price available from Hach Chemical Company, P.O. 
Box 389, Loveland, Colorado 80537. Table IB, Note 21.
    (22) OIC Chemical Oxygen Demand Method, 1978. Method and price 
available from Oceanography International Corporation, 512 West Loop, 
P.O. Box 2980, College Station, Texas 77840. Table IB, Note 20.
    (23) ORION Research Instruction Manual, Residual Chlorine Electrode 
Model 97-70, 1977. Method and price available from ORION Research 
Incorporation, 840 Memorial Drive, Cambridge, Massachusetts 02138. 
Table IB, Note 22.
    (24) Bicinchoninate Method for Copper. Method 8506, Hach Handbook 
of Water Analysis, 1979. Method and price available from Hach Chemical 
Company, P.O. Box 300, Loveland, Colorado 80537. Table IB, Note 25.
    (25) Hydrogen Ion (pH) Automated Electrode Method, Industrial 
Method Number 378-75WA. October 1976. Bran & Luebbe (Technicon) Auto 
Analyzer II. Method and price available from Bran & Luebbe Analyzing 
Technologies, Inc. Elmsford, N.Y. 10523. Table IB, Note 26.
    (26) 1,10-Phenanthroline Method using FerroVer Iron Reagent for 
Water, Hach Method 8008, 1980. Method and price available from Hach 
Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, 
Note 27.
    (27) Periodate Oxidation Method for Manganese, Method 8034, Hach 
Handbook for Water Analysis, 1979. Method and price available from Hach 
Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, 
Note 31.
    (28) Nitrogen, Nitrite-Low Range, Diazotization Method for Water 
and Wastewater, Hach Method 8507, 1979. Method and price available from 
Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table 
IB, Note 32.
    (29) Zincon Method for Zinc, Method 8009, Hach Handbook for Water 
Analysis, 1979. Method and price available from Hach Chemical Company, 
P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 38.
    (30) ``Direct Determination of Elemental Phosphorus by Gas-Liquid 
Chromatography,'' by R.F. Addison and R.G. Ackman, Journal of 
Chromatography, Volume 47, No. 3, pp. 421-426, 1970. Available in most 
public libraries. Back volumes of the Journal of Chromatography are 
available from Elsevier/North-Holland,Inc., Journal Information Center, 
52 Vanderbilt Avenue, New York, NY 10164. Cost available from 
publisher, Table IB, Note 36.
    (31) ``Direct Current Plasma (DCP) Optical Emission Spectrometric 
Method for Trace Elemental Analysis of Water and Wastes'', Method AES 
0029, 1986-Revised 1991. Fison Instruments, Inc., 32 Commerce Center, 
Cherry Hill Drive, Danvers, MA 01923. Table IB, Note 16.
    (32) ``Closed Vessel Microwave Digestion of Wastewater Samples for 
Determination of Metals, CEM Corporation, P.O. Box 200, Matthews, North 
Carolina 28106-0200, April 16, 1992. Available from the CEM 
Corporation. Table IB, Note 6.
    (33) Reserved.
    (34) ``Organochlorine Pesticides and PCB's in Wastewater Using 
EmporeTM Disk'', Test Method 3M 0222, Revised 10/28/94. 3M 
Corporation, 3M Center Building 220-9E-10, St. Paul, MN 55144-1000. 
Method available from 3M Corporation. Tables IC and ID, Note 9.
    (35) ``Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, 
Steam Distillation, Titrimetric Detection)'', revised 12/22/94, Perstop 
Analytical. Method available from Perstorp Analytical Corporation, P.O. 
Box 648, Wilsonville, OR 97070. Table IB, Note 28.
    (36) ``Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, 
Steam Distillation, Colorimetric Detection)'', revised 12/22/94, 
Perstop Analytical. Method available from Perstorp Analytical 
Corporation, P.O. Box 648, Wilsonville, OR 97070. Table IB, Note 29.
    (37) ``Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, 
Automated FIA Gas Diffusion)'', revised 12/22/94, Perstop Analytical. 
Method available from Perstorp Analytical Corporation, P.O. Box 648, 
Wilsonville, OR 97070. Table IB, Note 30.
    (38) Methods for the Determination of Metals in Environmental 
Samples, Environmental Monitoring Systems Laboratory, Office of 
Research and Development, U.S. Environmental Protection Agency, 
Cincinnati, OH 45268, EPA 600 R-94/111, May 1994. Table IB, Notes 1 and 
5.
    (39) ``Methods for the Determination of Inorganic Substances in 
Environmental Samples'', Environmental Monitoring Systems Laboratory, 
Office of Research and Development, U.S. Environmental Protection 
Agency, Cincinnati, OH 45268, Revised EPA 600 R-93/100 August 1993. 
Table IB, Note 1.
    (40) ``Standard Methods for the Examination of Water and 
Wastewater'', American Public Health Association, American Water Works 
Association, Water Environment Federation, 18th Edition Supplement, 
1994. Table IB, Note 23.
    5. Section 136.3 (e) is proposed to be amended by revising Table II 
to read as follows:


136.3  Identification of test procedures.

* * * * *
    (e) * * *

                                                                                                                                                                                                

[[Page 54003]]
                   Table II.--Required Containers, Preservation Techniques, and Holding Times                   
----------------------------------------------------------------------------------------------------------------
 Test procedure table parameter                                                                Maximum holding  
           number/name                  Container\1\         Preservation procedure\2\-\4\         time\5\      
----------------------------------------------------------------------------------------------------------------
                                           Table IA--Biological Tests                                           
                                                                                                                
----------------------------------------------------------------------------------------------------------------
1. Coliform (fecal).............  P,G                       a,b\6\                          6 hours.            
2. Coliform (fecal), Pres. of     P,G                       a,b\6\                          6 hours.            
 chlorine.                                                                                                      
3. Coliform (total).............  P,G                       a,b\6\                          6 hours.            
4. Coliform (total), Pres. of     P,G                       a,b\6\                          6 hours.            
 chlorine.                                                                                                      
5. Fecal streptococci...........  P,G                       a,b\6\                          6 hours.            
                                                                                                                
----------------------------------------------------------------------------------------------------------------
                                            Table IB--Inorganic Tests                                           
                                                                                                                
----------------------------------------------------------------------------------------------------------------
1. Acidity......................  P,G                       a                               14 days.            
2. Alkalinity...................  P,G                       a                               14 days.            
3. Aluminum\7\..................  P,G                       c                               6 months.           
4. Ammonia......................  P,G                       a,d                             28 days.            
5. Antimony\7\..................  P,G                       c                               6 months.           
6. Arsenic\7\...................  P,G                       c                               6 months.           
7. Barium\7\....................  P,G                       c                               6 months.           
8. Beryllium\7\.................  P,G                       c                               6 months.           
9. Biochemical oxygen demand      P,G                       a                               48 hours.           
 (BOD).                                                                                                         
10. Boron\7\....................  P,G                       c                               6 months.           
11. Bromide.....................  P,G                       e                               28 days.            
12. Cadmium\7\..................  P,G                       c                               6 months.           
13. Calcium\7\..................  P,G                       c                               6 months.           
14. Carbonaceous biochemical      P,G                       a                               48 hours.           
 oxygen demand (CBOD).                                                                                          
15. Chemical oxygen demand (COD)  P,G                       a,d                             28 days.            
16. Chloride....................  P,G                       e                               28 days.            
17. Chlorine....................  P,G                       e                               Immediate.          
18. Chromium VI (dissolved).....  P,G                       a                               24 hours.           
19. Chromium\7\.................  P,G                       c                               6 months.           
20. Cobalt\7\...................  P,G                       c                               6 months.           
21. Color.......................  P,G                       a                               48 hours.           
22. Copper\7\...................  P,G                       c                               6 months.           
23. Cyanide.....................  P,G                       a,f\6\,g                        14 days.\8\         
24. Cyanide amenable............  P,G                       a,f\6\,g                        14 days.\8\         
25. Fluoride....................  P                         e                               28 days.            
26. Gold\7\.....................  P,G                       c                               6 months.           
27. Hardness....................  P,G                       c or d                          6 months.           
28. Hydrogen ion (pH)...........  P,G                       e                               Immediate.          
29. Iridium\7\..................  P,G                       c                               6 months.           
30. Iron\7\.....................  P,G                       c                               6 months.           
31. Kjeldahl nitrogen...........  P,G                       a,d                             28 days.            
32. Lead\7\.....................  P,G                       c                               6 months.           
33. Magnesium\7\................  P,G                       c                               6 months.           
34. Manganese\7\................  P,G                       c                               6 months.           
35. Mercury.....................  P,G                       c                               28 days.            
36. Molybdenum\7\...............  P,G                       c                               6 months.           
37. Nickel\7\...................  P,G                       c                               6 months.           
38. Nitrate.....................  P,G                       a                               48 hours.           
39. Nitrate-nitrite.............  P,G                       a,d                             28 days.            
40. Nitrite.....................  P,G                       a                               48 hours.           
41. Oil and grease..............  G                         a; d or h                       28 days.            
42. Organic carbon..............  P,G                       a; d or h or i                  28 days.            
43. Organic nitrogen............  P,G                       a,d                             28 days.            
44. Orthophosphate..............  P,G                       a,j                             48 hours.           
45. Osmium\7\...................  P,G                       c                               6 months.           
46. Oxygen, dissolved:                                                                                          
    By probe....................  G                         e                               Immediate.          
    By winkler..................  G bottle and top          k                               8 hours. 4          
47. Palladium\7\................  P,G                       c                               6 months.           
48. (Reserved)..................  ........................  ..............................  ....................
49. Phenols.....................  G                         a,d                             28 days.            
50. Phosphorus (elemental)......  G                         a                               48 hours.           
51. Phosphorus..................  P,G                       a,d                             28 days.            
52. Platinum\7\.................  P,G                       c                                6 months.          
53. Potassium\7\................  P,G                       c                               6 months.           
54. Residue, total..............  P,G                       a                               7 days.             
55. Residue, filterable.........  P,G                       a                               7 days.             
56. Residue, nonfilterable (TSS)  P,G                       a                               7 days.             
57. Residue, settleable.........  P,G                       a                               48 hours.           
58. Residue, Volatile...........  P,G                       a                               7 days.             

[[Page 54004]]
                                                                                                                
59. Rhodium\7\..................  P,G                       c                               6 months.           
60. Ruthenium\7\................  P,G                       c                               6 months.           
61. Selenium\7\.................  P,G                       c                               6 months.           
62. Silica\7\...................  P                         a                               28 days.            
63. Silver\7\...................  P,G                       c                               6 months.           
64. Sodium\7\...................  P,G                       c                               6 months.           
65. Specific conductance........  P,G                       a                               28 days.            
66. Sulfate.....................  P,G                       a                               28 days.            
67. Sulfide.....................  P,G                       a,l,m                           7 days.             
68. Sulfite.....................  P,G                       e                               Immediate.          
69. Surfactants.................  P,G                       a                               48 hours.           
70. Temperature.................  P,G                       e                               Immediate.          
71. Thallium\7\.................  P,G                       c                               6 months.           
72. Tin\7\......................  P,G                       c                               6 months.           
73. Titanium\7\.................  P,G                       c                               6 months.           
74. Turbidity...................  P,G                       a                               48 hours.           
75. Vanadium\7\.................  P,G                       c                               6 months.           
76. Zinc\7\.....................  P,G                       c                               6 months.           
----------------------------------------------------------------------------------------------------------------
                                Table IC--Non-Pesticide Organic Compounds\9\,\10\                               
                                                                                                                
----------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................  G,T                       a,b\6\,n                        7 days.\11\         
2. Acenaphthylene...............  G,T                       a,b\6\,n                        7 days.\11\         
3. Acrolein.....................  G,T                       a,o\6\,p                        14 days.\12\        
4. Acrylonitrile................  G,T                       a,o\6\                          14 days.            
5. Anthracene...................  G,T                       a,b\6\,n                        7 days.\11\         
6. Benzene......................  G,T                       a,h,o\6\                        14 days.            
7. Benzidine....................  G,T                       a,b\6\,\13\                     7 days.\14\         
8. Benzo(a)anthracene...........  G,T                       a,b\6\,n                        7 days.\11\         
9. Benzo(a)pyrene...............  G,T                       a,b\6\,n                        7 days.\11\         
10. Benzo(b)fluoranthene........  G,T                       a,b\6\,n                        7 days.\11\         
11. Benzo(g,h,i)perylene........  G,T                       a,b\6\,n                        7 days.\11\         
12. Benzo(k)fluoranthene........  G,T                       a,b\6\,n                        7 days.\11\         
13. Benzyl chloride.............  G,T                       a,o\6\                          14 days.            
14. Benzyl butyl phthalate......  G,T                       a                               7 days.\11\         
15. Bis(2-chloroethoxy) methane.  G,T                       a,b\6\                          7 days.\11\         
16. Bis(2-chloroethyl) ether....  G,T                       a,b\6\                          7 days.\11\         
17. Bis(2-ethylhexyl) phthalate.  G,T                       a                               7 days.\11\         
18. Bromodichloromethane........  G,T                       a,o\6\                          14 days.            
19. Bromoform...................  G,T                       a,o\6\                          14 days.            
20. Bromomethane................  G,T                       a,o\6\                          14 days.            
21. 4-Bromophenylphenyl ether...  G,T                       a,b\6\                          7 days.\11\         
22. Carbon tetrachloride........  G,T                       a,o\6\                          14 days.            
23. 4-Chloro-3-methylphenol.....  G,T                       a,b\6\                          7 days.\11\         
24. Chlorobenzene...............  G,T                       a,o\6\                          14 days.            
25. Chloroethane................  G,T                       a,o\6\                          14 days.            
26. 2-Chloroethylvinyl ether....  G,T                       a,o\6\                          14 days.            
27. Chloroform..................  G,T                       a,o\6\                          14 days.            
28. Chloromethane...............  G,T                       a,o\6\                          14 days.            
29. 2-Chloronaphthalene.........  G,T                       a                               7 days.\11\         
30. 2-Chlorophenol..............  G,T                       a,b\6\                          7 days.\11\         
31. 4-Chlorophenylphenyl ether..  G,T                       a,b\6\                          7 days.\11\         
32. Chrysene....................  G,T                       a,b\6\,n                        7 days.\11\         
33. Dibenzo(a,h)anthracene......  G,T                       a,b\6\,n                        7 days.\11\         
34. Dibromochloromethane........  G,T                       a,o\6\                          14 days.            
35. 1,2-Dichlorobenzene.........  G,T                       a,o\6\                          14 days.            
36. 1,3-Dichlorobenzene.........  G,T                       a,o\6\                          14 days.            
37. 1,4-Dichlorobenzene.........  G,T                       a,h,o\6\                        14 days.            
38. 3,3-Dichlorobenzidine.......  G,T                       a,b\6\                          7 days.\13\         
39. Dichlorodifluoromethane.....  G,T                       a,o\6\                          14 days.            
40. 1,1-Dichloroethane..........  G,T                       a,o\6\                          14 days.            
41. 1,2-Dichloroethane..........  G,T                       a,o\6\                          14 days.            
42. 1,1-Dichloroethene..........  G,T                       a,o\6\                          14 days.            
43. trans-1,2-Dichloroethene....  G,T                       a,o\6\                          14 days.            
44. 2,4-Dichlorophenol..........  G,T                       a,b\6\                          7 days.\11\         
45. 1,2-Dichloropropane.........  G,T                       a,o\6\                          14 days.            
46. cis-1,3-Dichloropropene.....  G,T                       a,o\6\                          14 days.            
47. trans-1,3-Dichloropropene...  G,T                       a,o\6\                          14 days.            
48. Diethyl phthalate...........  G,T                       a                               7 days.\11\         
49. 2,4-Dimethylphenol..........  G,T                       a,b\6\                          7 days.\11\         
50. Dimethyl phthalate..........  G,T                       a                               7 days.\11\         

[[Page 54005]]
                                                                                                                
51. Di-n-butyl phthalate........  G,T                       a                               7 days.\11\         
52. Di-n-octyl phthalate........  G,T                       a                               7 days.\11\         
53. 2,4-Dinitrophenol...........  G,T                       a,b\6\                          7 days.\11\         
54. 2,4-Dinitrotoluene..........  G,T                       a,b\6\,n                        7 days.\11\         
55. 2,6-Dinitrotoluene..........  G,T                       a,b\6\,n                        7 days.\11\         
56. Epichlorohydrin.............  G,T                       a,o\6\                          14 days.            
57. Ethylbenzene................  G,T                       a,h,o\6\                        14 days.            
58. Fluoranthene................  G,T                       a,b\6\,n                        7 days.\11\         
59. Fluorene....................  G,T                       a,b\6\,n                        7 days.\11\         
60. Hexachlorobenzene...........  G,T                       a                               7 days.\11\         
61. Hexachlorobutadiene.........  G,T                       a                               7 days.\11\         
62. Hexachlorocyclopentadiene...  G,T                       a,b\6\                          7 days.\11\         
63. Hexachloroethane............  G,T                       a,b\6\                          7 days.\11\         
64. Ideno(1,2,3-cd)pyrene.......  G,T                       a,b\6\,n                        7 days.\11\         
65. Isophorone..................  G,T                       a,b\6\,n                        7 days.\11\         
66. Methylene chloride..........  G,T                       a,o\6\                          14 days.            
67. 2-Methyl-4,6-dinitrophenol..  G,T                       a,b\6\                          7 days,\11\         
68. Naphthalene.................  G,T                       a,b\6\,n                        7 days.\11\         
69. Nitrobenzene................  G,T                       a,b\6\,n                        7 days.\11\         
70. 2-Nitrophenol...............  G,T                       a,b\6\                          7 days.\11\         
71. 4-Nitrophenol...............  G,T                       a,b\6\                          7 days.\11\         
72. N-Nitrosodimethylamine......  G,T                       a,b\6\,n                        7 days.\11\         
73. N-Nitrosodi-n-propylamine...  G,T                       a,b\6\,n                        7 days.\11\         
74. N-Nitrosodiphenylamine......  G,T                       a,b\6\,n\15\                    7 days.\11\         
75. 2,2-Oxybis(1-chloropropane).  G,T                       a,b\6\                          7 days.\11\         
76. PCB-1016....................  G,T                       a,b\6\                          7 days.\11\         
77. PCB-1221....................  G,T                       a,b\6\                          7 days.\11\         
78. PCB-1232....................  G,T                       a,b\6\                          7 days.\11\         
79. PCB-1242....................  G,T                       a,b\6\                          7 days.\11\         
80. PCB-1248....................  G,T                       a,b\6\                          7 days.\11\         
81. PCB-1254....................  G,T                       a,b\6\                          7 days.\11\         
82. PCB-1260....................  G,T                       a,b\6\                          7 days.\11\         
83. Pentachlorophenol...........  G,T                       a,b\6\                          7 days.\11\         
84. Phenanthrene................  G,T                       a,b\6\,n                        7 days.\11\         
85. Phenol......................  G,T                       a,b\6\                          7 days.\11\         
86. Pyrene......................   G,T                      a,b\6\,n                        7 days.\11\         
87. 2,3,7,8-Tetrachlorodibenzo-p- G,T                       a,b\6\                          7 days.\11\         
 dioxin.                                                                                                        
88. 1,1,2,2-Tetrachloroethane...  G,T                       a,o\6\                          14 days.            
89. Tetrachloroethene...........  G,T                       a,o\6\                          14 days.            
90. Toluene.....................  G,T                       a,h,o\6\                        14 days.            
91. 1,2,4-Trichlorobenzene......  G,T                       a,o\6\                          14 days.            
92. 1,1,1-Trichloroethane.......  G,T                       a,o\6\                          14 days.            
93. 1,1,2-Trichloroethane.......  G,T                       a,o\6\                          14 days.            
94. Trichloroethene.............  G,T                       a,o\6\                          14 days.            
95. Trichlorofluoromethane......  G,T                       a,o\6\                          14 days.            
96. 2,4,6-Trichlorophenol.......  G,T                       a,b\6\                          7 days.\11\         
97. Vinyl chloride..............  G,T                       a,o\6\                          14 days.            
----------------------------------------------------------------------------------------------------------------
                                          Table ID--Pesticides\9\,\10\                                          
                                                                                                                
----------------------------------------------------------------------------------------------------------------
1-70. Pesticides................  G,T                       a,q\16\                         7 days.\11\         
                                                                                                                
----------------------------------------------------------------------------------------------------------------
                                           Table IE--Radiologic Tests                                           
                                                                                                                
----------------------------------------------------------------------------------------------------------------
1-5. Alpha, beta and radium.....  P,G                       c                               6 months.           
----------------------------------------------------------------------------------------------------------------
Table II Notes                                                                                                  
                                                                                                                
\1\Container abbreviations: P = Polyethylene, G = Glass and T = PTFE-lined cap or septum.                       
\2\Sample preservation should be performed immediately upon sample collection. For composite chemical samples   
  each aliquot should be preserved at the time of collection. When use of an automated sampler makes it         
  impossible to preserve each aliquot, then chemical samples may be preserved by maintaining at 4 deg.C until   
  compositing and sample splitting is completed.                                                                
\3\Procedure abbreviations:                                                                                     
  a: Cool 4 deg.C                                                                                               
  b: 0.008% Na2S2O3\6\                                                                                          
  c: HNO3 to pH<2                                                                                               
  d: H2SO4 to pH<2                                                                                              
  e: None required                                                                                              
  f: 0.6 g ascorbic acid\6\                                                                                     
  g: NaOH to pH>12                                                                                              
  h: HCl to pH<2                                                                                                
  i: H3PO4 to pH <2                                                                                             
  j: Filter immediately                                                                                         

[[Page 54006]]
                                                                                                                
  k: Fix on site and store in dark                                                                              
  l: Add zinc acetate                                                                                           
  m: NaOH to pH>9                                                                                               
  n: Store in dark                                                                                              
  o: 0.025 g ascorbic acid\6\                                                                                   
  p: Adjust pH to 4-5\10\                                                                                       
  q: Adjust pH to 5-9                                                                                           
\4\When any sample is to be shipped by common carrier or sent through the United States Mails, it must comply   
  with the Department of Transportation Hazardous Materials Regulations (49 CFR part 172). The person offering  
  such material for transportation is responsible for ensuring such compliance. For the preservation            
  requirements of Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of   
  Transportation has determined that the Hazardous Materials Regulations do not apply to the following          
  materials: Hydrochloric acid (HCl) in water solutions at concentrations of 0.04% by weight or less (pH about  
  1.96 or greater); Nitric acid (HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about
  1.62 or greater); Sulfuric acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH   
  about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight  
  or less (pH about 12.30 or less).                                                                             
\5\Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that 
  samples may be held before analysis and still be considered valid. Samples may be held for longer periods only
  if the permittee, or monitoring laboratory, has data on file to show that for the specific types of samples   
  under study, the analytes are stable for the longer time, and has received a variance from the Regional       
  Administrator under Sec. 136.3(e). Some samples may not be stable for the maximum time period given in the    
  table. A permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge 
  exists to show that this is necessary to maintain sample stability. See Sec. 136.3(e) for details. The term   
  ``analyze immediately'' usually means within 15 minutes or less of sample collection.                         
\6\Should only be used in the presence of residual chlorine.                                                    
\7\Samples should be filtered immediately on-site before adding preservative for dissolved metals.              
\8\Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead     
  acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can
  be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is    
  filtered and then NaOH is added to pH 12.                                                                     
\9\Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.                       
\10\When samples are to be extracted and analyzed for multiple analytes, the most stringent preservation        
  procedures and shortest maximum holding times should be observed for optimum safeguard of sample integrity.   
  Samples extracted for a wide range of analytes may be preserved by cooling to 4 deg.C, reducing residual      
  chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved  
  in this manner may be held for seven days before extraction and for forty days after extraction. Exceptions to
  this optional preservation and holding time procedure are noted in footnotes 6,13, and 14.                    
\11\Samples must be extracted within seven days of collection. The extract must be analyzed within 40 days of   
  extraction.                                                                                                   
\12\Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling.                 
\13\If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 0.2 to     
  prevent rearrangement to benzidine.                                                                           
\14\Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)   
  atmosphere.                                                                                                   
\15\Adjust pH to 7-10 with NaOH within 24 hours of sampling.                                                    
\16\The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are     
  extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% N2S2O3.                       



Appendices C and D--[Removed]

    6. In Part 136, Appendices C and D are proposed to be removed.

[FR Doc. 95-25775 Filed 10-17-95; 8:45 am]
BILLING CODE 6560-50-P