[Federal Register Volume 60, Number 64 (Tuesday, April 4, 1995)]
[Rules and Regulations]
[Pages 17160-17169]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 95-5022]
[[Page 17159]]
_______________________________________________________________________
Part IV
Environmental Protection Agency
_______________________________________________________________________
40 CFR Part 136
_______________________________________________________________________
Guidelines Establishing Test Procedures for the Analysis of Pollutants
Under the Clean Water Act, Technical Amendments; Final Rule
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules
and Regulations
[[Page 17160]]
ENVIRONMENTAL PROTECTION AGENCY
40 CFR Part 136
[FRL-5162-7]
Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the Clean Water Act; Technical Amendments
AGENCY: Environmental Protection Agency (EPA).
ACTION: Final rule: Technical amendments.
-----------------------------------------------------------------------
SUMMARY: This action under the Clean Water Act (CWA) section 304(h)
amends 40 CFR Part 136 to add clarifying footnotes to the lists of
approved test procedures, to update method citations in Tables IA, IB,
IC, and ID, to amend the incorporation by reference section of the
regulation accordingly, and to correct certain typographical errors and
omissions in the Technical Amendments appearing in the Federal Register
of January 31, 1994.
EFFECTIVE DATE: This amendment becomes effective on May 4, 1995. The
incorporation by reference of the publications listed in this document
are approved by the Director of Federal Register as of May 4, 1995.
FOR FURTHER INFORMATION CONTACT: James E. Longbottom, Environmental
Monitoring Systems Laboratory, Office of Research and Development, U.S.
Environmental Protection Agency, Cincinnati, Ohio 45268, Telephone
Number: (513) 569-7308.
SUPPLEMENTARY INFORMATION:
I
These technical amendments update and/or correct errors and
inadvertent omissions in the references to analytical methods already
approved under section 304(h) to the current editions published by EPA,
U.S. Geological Survey, Standard Methods for the Examination of Water
and Wastewater (Standard Methods), the American Society for Testing and
Materials (ASTM), and the Association of Official Analytical Chemists
(AOAC) International. No new methods are introduced. EPA has carefully
reviewed each approved method for substantive changes between the
current editions and the previously approved editions. Methods cited in
this amendment that were not previously cited are substantively the
same as the approved EPA method and/or were derived from the EPA
method.
II
References in Table IB, to the American Society for Testing and
Materials (ASTM), have also been updated and corrected where
appropriate to the 1994 edition. Several ASTM methods are no longer
cited because they have been discontinued by ASTM and are not included
in the 1994 Standards book.
III
The remaining amendments in this notice are very minor and are
typographical or editorial in nature. The parts of Tables IA, IC and
ID, and certain notes to Tables IB, IC, and ID where reference updates,
corrections, and clarifications have been made are reprinted in this
notice for the information and use of the regulated community. Table IB
has been reprinted in its entirety for the convenience of the user.
Unless otherwise indicated in this notice, the methods contained in
the Standard Methods 18th edition and the ASTM Standards 1994 edition
are previously approved methods that were reballoted without technical
change or were not reballoted. Any changes are editorial,
typographical, or grammatical.
IV Regulatory Requirements
A. Executive Order 12866
Under Executive Order 12866, EPA must determine whether a
regulation is ``major'' and, therefore, requires a regulatory impact
analysis. EPA has determined that these technical amendments are not
major as they 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. These amendments simply
specify analytical techniques which may be used by laboratories in
measuring concentrations of certain analytes and, therefore, have no
adverse economic impacts.
B. Administrative Procedure Act
The Administrative Procedure Act, 5 U.S.C. 553 (b)(B), authorizes
an agency to forego notice and comment rulemaking when the agency for
good cause finds that notice and public procedure thereon are
impracticable, unnecessary or contrary to the public interest. EPA
believes that public comment on the foregoing technical amendments is
unnecessary because the updates to method references do not change the
methods contained therein. In publishing the new editions of their test
protocols, ASTM and Standard Methods have balloted these methods for
reapproval without technical change or the methods were republished as
unballoted. Additionally, the typographical errors corrected in the CFR
do not amend substantive requirements. Therefore, notice and public
procedure is unnecessary and does not apply to this Technical Amendment
Notice.
C. Regulatory Flexibility Act
This amendment is consistent with the objectives of the Regulatory
Flexibility Act (5 U.S.C. 602 et seq.) because it will not have a
significant economic impact on a substantial number of small entities.
The procedures cited in this rule give all laboratories the flexibility
to use these procedures or already approved alternative procedures.
D. Paperwork Reduction Act
This rule contains no request 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.
List of Subjects in 40 CFR Part 136
Environmental protection, Incorporation by reference, Reporting and
recordkeeping requirements, Water pollution control.
Dated: February 15, 1995.
Joseph K. Alexander,
Acting Assistant Administrator for Research and Development, U.S.
Environmental Protection Agency.
40 CFR part 136 is amended 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) Pub. L. 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 is amended as follows:
a. In paragraph (a) by revising entries 1 and 2 of Table IA, Table
IB, entries 33 and 37 and Notes 3 and 5a of Table IC, entries 8,
9, 10, and 22 and Note 5 of Table ID;
b. In paragraph (b) by revising Reference 10; and
c. In paragraph (e), in table II, under ``Table IB-Inorganic
Tests:'' by revising entry 10 and under ``Metals:'' by revising entries
``3, 5-8, 12, 13, 19, 20, 22, 26, 29, 30, 32-34, 36, 37, 45, 47, 51,
52, 58-60, 62, 63, 70-72, 74, 75. Metals, [[Page 17161]] except boron,
chromium VI and mercury'', 42 and 61, to read as follows:
Sec. 136.3 Identification of test procedures.
(a) * * *
Table IA.--List of Approved Biological Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method No. or page)
-----------------------------------------------------------------
Parameter, units and method Method\1\ Standard methods
EPA\2\ 18th ed. ASTM USGS\3\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number per 100 mL.. Most Probable Number (MPN), 5 tube, 3 p. 132...... 9221C and E......
dilution.
Membrane filter (MF)\4\, single step.... p. 124...... 9222D ................ B-0050-85
2. Coliform (fecal) in presence of MPN, 5 tube, 3 dilution................. p. 132...... 9221C and E...... ................ .............
chlorine, number per 100 mL. MF\4\, single step\5\................... p. 124...... 9222D
* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IA Notes:
\1\The method used must be specified when results are reported.
\2\Bordner, R.H., and J.A. Winter, eds. 1978. ``Microbiological Methods for Monitoring the Environment, Water and Waste''. Environmental Monitoring
Systems Laboratory, U.S. Environmental Protection Agency. EPA-600/8-78-017.
\3\Britton, L.J., and P.E. Greeson, P.E., eds., 1989. ``Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples,''
Techniques of Water Resources Investigations of the U.S. Geological Survey, Techniques of Water Resources Investigations, Book 5, Chapter A4,
Laboratory Analysis, U.S. Geological Survey, U.S. Department of Interior, Reston, Virginia.
\4\A 0.45 m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated, and to be free of
extractables which could interfere with their growth.
\5\Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
Table IB.--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
Parameter, units and method --------------------------------------------------------------------------------------------------------------------
EPA1,35 STD methods 18th ed. ASTM USGS\2\ Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:
Electrometric endpoint or 305.1 2310 B(4a).............. D1067-92
phenolphthalein endpoint.
2. Alkalinity, as CaCO3, mg/L:
Electrometric or Colorimetric 310.1 2320 B.................. D1067-92.................... I-1030-85............... 973.43.\3\
titration to pH 4.5, manual or 310.2 ........................ ............................ I-2030-85
automated.
3. Aluminum--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 202.1 3111 D.................. ............................ I-3051-85
AA furnace..................... 202.2 3113 B
Inductively Coupled Plasma/ \5\200.7 3120 B
Atomic Emission Spectrometry
(ICP/AES)\36\.
Direct Current Plasma (DCP)\36\ ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Eriochrome ........... 3500-Al D
cyanine R).
4. Ammonia (as N), mg/L:
Manual, distillation (at pH 350.2 4500-NH3 B.............. ............................ ........................ 973.49.\3\
9.5),\6\ followed by.
Nesslerization................. 350.2 4500-NH3 C.............. D1426-93(A)................. I-3520-85............... 973.49.\3\
Titration...................... 350.2 4500-NH3 E
Electrode...................... 350.3 4500-NH3 F or G......... D1426-93(B)
Automated phenate, or.......... 350.1 4500-NH3 H.............. ............................ I-4523-85
Automated electrode............ ........... ........................ ............................ ........................ Note 7.
5. Antimony-Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 204.1 3111 B
AA furnace..................... 204.2 3113 B
ICP/AES\36\.................... \5\200.7 3120 B
6. Arsenic-Total,\4\ mg/L:
Digestion\4\ followed by....... 206.5
AA gaseous hydride......... 206.3 3114 B 4.d.............. D2972-93(B)................. I-3062-85
AA furnace................. 206.2 3113 B.................. D2972-93(C)
[[Page 17162]]
ICP/AES,\36\ or............ \5\200.7 3120 B
Colorimetric (SDDC)........ 206.4 3500-As C............... D2972-93(A)................. I-3060-85
7. Barium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 208.1 3111 D.................. ............................ I-3084-85
AA furnace..................... 208.2 3113 B.................. D4382-91
ICP/AES\36\.................... \5\200.7 3120 B
DCP\36\........................ ........... ........................ ............................ ........................ Note 34.
8. Beryllium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 210.1 3111 D.................. D3645-93(88)(A)............. I-3095-85
AA furnace..................... 210.2 3113 B.................. D3645-93(88)(B)
ICP/AES........................ \5\200.7 3120 B
DCP, or........................ ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (aluminon)........ ........... 3500-Be D
9. Biochemical oxygen demand
(BOD5), mg/L:
Dissolved Oxygen Depletion..... 405.1 5210 B.................. ............................ I-1578-78\8\............ 973.44,\3\ p. 17.\9\
10. Boron\37\--Total, mg/L:
Colorimetric (curcumin)........ 212.3 4500-B B................ ............................ I-3112-85
ICP/AES, or.................... \5\200.7 3120 B
DCP............................ ........... ........................ D4190-82(88)................ ........................ Note 3.\4\
11. Bromide, mg/L:
Titrimetric.................... 320.1 ........................ D1246-82(88)(C)............. I-1125-85............... p. S44.\10\
12. Cadmium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 213.1 3111 B or C............. D3557-90(A or B)............ I-3135-85 or I-3136-85.. 974.27,\3\ p. 37.\9\
AA furnace..................... 213.2 3113 B.................. D3557-90(D)
ICP/AES\36\.................... \5\200.7 3120 B.................. ............................ I-1472-85
DCP\36\........................ ........... ........................ D4190-82(88)................ ........................ Note 34.
Voltametry,\11\ or............. ........... ........................ D3557-90(C)
Colorimetric (Dithizone)....... ........... 3500-Cd D
13. Calcium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 215.1 3111 B.................. D511-93(B).................. I-3152-85
ICP/AES........................ \5\200.7 3120 B
DCP, or........................ ........... ........................ ............................ ........................ Note 34.
Titrimetric (EDTA)............. 215.2 3500-Ca D............... D511-93(A)
14. Carbonaceous biochemical oxygen
demand (CBOD5), mg/L\12\:
Dissolved Oxygen Depletion with ........... 5210 B
nitrification inhibitor.
15. Chemical oxygen demand (COD), 410.1 5220 C.................. D1252-88(A)................. I-3560-85............... 973.46,\3\ p. 17.\9\
mg/L; Titrimetric, or. 410.2 ........................ ............................ I-3562-85...............
410.3
Spectrophotometric, manual or 410.4 5220 D.................. D1252-88(B)................. I-3561-85............... Notes 13 or 14.
automated.
16. Chloride, mg/L:
Titrimetric (silver nitrate) or ........... 4500-Cl- B.............. D512-89(B).................. I-1183-85
(Mercuric nitrate)............. 325.3 4500-Cl- C.............. D512-89(A).................. I-1184-85............... 973.51.\3\
Colorimetric, manual or........ ........... ........................ ............................ I-1187-85
Automated (Ferricyanide)....... 325.1 or 4500-Cl- E.............. ............................ I-2187-85
325.2
17. Chlorine--Total residual, mg/L;
Titrimetric:
Amperometric direct............ 330.1 4500-Cl D............... D1253-86(92)
Iodometric direct.............. 330.3 4500-Cl B
Back titration ether end- 330.2 4500-Cl C
point\15\ or.
DPD-FAS........................ 330.4 4500-Cl F
Spectrophotometric, DPD........ 330.5 4500-Cl G
Or Electrode................... ........... ........................ ............................ ........................ Note 16.
18. Chromium VI dissolved, mg/L;
0.45 micron filtration followed
by:
AA chelation-extraction or..... 218.4 3111 C.................. ............................ I-1232-85
Colorimetric ........... 3500-Cr D............... D1687-92(A)................. I-1230-85
(Diphenylcarbazide).
19. Chromium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 218.1 3111 B.................. D1687-92(B)................. I-3236-85............... 974.27.\3\
[[Page 17163]]
AA chelation-extraction........ 218.3 3111 C
AA furnace..................... 218.2 3113 B.................. D1687-92(C)
ICP/AES\36\.................... \5\200.7 3120 B
DCP,\36\ or.................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric ........... 3500-Cr D
(Diphenylcarbazide)
20. Cobalt--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 219.1 3111 B or C............. D3558-90(A or B)............ I-3239-85............... p. 37.\9\
AA furnace..................... 219.2 3113 B.................. D3558-90(C)
ICP/AES........................ \5\200.7 3120 B
DCP............................ ........... ........................ D4190-82(88)................ ........................ Note 34.
21. Color platinum cobalt units or
dominant wavelength, hue,
luminance purity:
Colorimetric (ADMI), or........ 110.1 2120 E.................. ............................ ........................ Note 18.
(Platinum cobalt), or.......... 110.2 2120 B.................. ............................ I-1250-85............... ....................
Spectrophotometric............. 110.3 2120 C
22. Copper--Total,4 mg/L;
Digestion4 followed by:
AA direct aspiration36......... 220.1 3111 B or C............. D1688-90(A or B)............ I-3270-85 or I3271-85... 974.273 p. 37.9
AA furnace..................... 220.2 3113 B.................. D1688-90(C)
ICP/AES36...................... 5200.7 3120 B
DCP36 or....................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Neocuproine) or.. ........... 3500-Cu D
(Bicinchoninate)............... ........... Or E.................... ............................ ........................ Note 19.
23. Cyanide--Total, mg/L:
Manual distillation with MgCl2 ........... 4500-CN C............... D2036-91(A)
followed by.
Titrimetric, or................ ........... 4500-CN D............... ............................ ........................ p. 22.9
Spectrophotometric, manual or.. 31335.2 4500-CN E............... D2036-91(A)................. I-3300-85
Automated20.................... 31335.3
24. Cyanide amenable to
chlorination,mg/L:
Manual distillation with MgCl2 335.1 4500-CN G............... D2036-91(B)
followed by titrimetric or
Spectrophotometric.
25. Fluoride--Total, mg/L:
Manual distillation6 followed ........... 4500-F B
by.
Electrode, manual or........... 340.2 4500-F C................ D1179-93(B)
Automated...................... ........... ........................ ............................ I-4327-85
Colorimetric (SPADNS).......... 340.1 4500-F D................ D1179-93(A)
Or Automated complexone........ 340.3 4500-F E
26. Gold--Total,4 mg/L; Digestion4
followed by:
AA direct aspiration........... 231.1 3111 B
AA furnace, or................. 231.2
DCP............................ ........... ........................ ............................ ........................ Note 34.
27. Hardness--Total, as CaCO3, mg/L
Automated colorimetric,........ 130.1
Titrimetric (EDTA), or Ca plus 130.2 2340 B or C............. D1126-86(92)................ I-1338-85............... 973.52B.3
Mg as their carbonates, by
inductively coupled plasma or
AA direct aspiration. (See
Parameters 13 and 33).
28. Hydrogen ion (pH), pH units
Electrometric measurement, or.. 150.1 4500-H+ B............... D1293-84(90)(A or B)........ I-1586-85............... 973.41.3
Automated electrode............ ........... ........................ ............................ ........................ Note 21.
29. Iridium--Total,4 mg/L;
Digestion4 followed by:
AA direct aspiration or........ 235.1 3111 B
AA furnace..................... 235.2
30. Iron--Total,4 mg/L; Digestion4
followed by:
AA direct aspiration36......... 236.1 3111 B or C............. D1068-90(A or B)............ I-3381-85............... 974.27.3
AA furnace..................... 236.2 3113 B.................. D1068-90(C)
ICP/AES36...................... 5200.7 3120 B
DCP36 or....................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Phenanthroline).. ........... 3500-Fe D............... D1068-90(D)................. ........................ Note 22.
[[Page 17164]]
31. Kjeldahl Nitrogen--Total, (as
N), mg/L
Digestion and distillation 351.3 4500-NH3 B or C......... D3590-89(A)
followed by.
Titration...................... 351.3 4500-NH3 E.............. D3590-89(A)................. ........................ 973.48.3
Nesslerization................. 351.3 4500-NH3 C.............. D3590-89(A)
Electrode...................... 351.3 4500-NH3 F or G
Automated phenate colorimetric. 351.1 ........................ ............................ I-4551-788
Semi-automated block digestor 351.2 ........................ D3590-89(B)
colorimetric, or.
Manual or block digestor 351.4 ........................ D3590-89(A)
Potentiometric.
32. Lead--Total,4 mg/L;
Digestion\4\ followed by:
AA direct aspiration36......... 239.1 3111 B or C............. D3559-90(A or B)............ I-3399-85............... 974.27.3
AA furnace..................... 239.2 3113 B.................. D3559-90(D)
ICP/AES36...................... 5200.7 3120 B
DCP36.......................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Voltametry11 or................ ........... ........................ D3559-90(C)
Colorimetric (Dithizone)....... ........... 3500-Pb D
33. Magnesium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 242.1 3111 B.................. D511-93(B).................. I-3447-85............... 974.27.\3\
ICP/AES........................ \5\200.7 3120 B
DCP, or........................ ........... ........................ ............................ ........................ Note 34.
Gravimetric.................... ........... 3500-Mg D
34. Manganese--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 243.1 3111 B.................. D858-90(A or B)............. I-3454-85............... 974.27.\3\
AA furnace..................... 243.2 3113 B.................. D858-90(C)
ICP/AES\36\.................... \5\200.7 3120 B
DCP\36\ or..................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Persulfate), or.. ........... 3500-Mn D............... ............................ ........................ 920.203.\3\
(Periodate).................... ........... ........................ ............................ ........................ Note 23.
35. Mercury--Total,\4\ mg/L:
Cold vapor, manual or.......... 245.1 3112 B.................. D3223-91.................... I-3462-85............... 977.22.\3\
Automated...................... 245.2
36. Molybdenum--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 246.1 3111 D.................. ............................ I-3490-85
AA furnace..................... 246.2 3113 B
ICP/AES........................ \5\200.7 3120 B
DCP............................ ........... ........................ ............................ ........................ Note 34.
37. Nickel--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 249.1 3111 B or C............. D1886-90(A or B)............ I-3499-85
AA furnace..................... 249.2 3113 B.................. D1886-90(C)
ICP/AES\36\.................... \5\200.7 3120 B
DCP\36\, or.................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (heptoxime)....... ........... 3500-Ni D
38. Nitrate (as N), mg/L:
Colorimetric (Brucine sulfate), 352.1 ........................ ............................ ........................ 973.50,\3\ 419
or Nitrate-nitrite N minus D,\17\ p. 28.\9\
Nitrite N (See parameters 39
and 40).
39. Nitrate-nitrite (as N), mg/L:
Cadmium reduction, Manual or... 353.3 4500-NO3- E............. D3867-90(B)
Automated, or.................. 353.2 4500-NO3- F............. D3867-90(A)................. I-4545-85
Automated hydrazine............ 353.1 4500-NO3- H
40. Nitrite (as N), mg/L;
Spectrophotometric:
Manual or...................... 354.1 4500-NO2- B............. ............................ ........................ Note 25.
Automated (Diazotization)...... ........... ........................ ............................ I-4540-85
41. Oil and grease--Total
recoverable, mg/L:
Gravimetric (extraction)....... 413.1 5520 B\38\
42. Organic carbon--Total (TOC), mg/
L:
Combustion or oxidation........ 415.1 5310 B, C, or D......... D2579-93 (A or B)........... ........................ 973.47,3 p. 14.24
43. Organic nitrogen (as N), mg/L:
[[Page 17165]]
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............... 973.56.3
Manual single reagent.......... 365.2 4500-P E................ D515-88(A) ........................ 973.55\3\.
Manual two reagent............. 365.3
45. Osmium--Total\4\, mg/L;
Digestion\4\ followed by:
AA direct aspiration, or....... 252.1 3111 D
AA furnace..................... 252.2
46. Oxygen, dissolved, mg/L:
Winkler (Azide modification), 360.2 4500-O C................ D888-92(A).................. I-1575-78\8\............ 973.45B.3
or.
Electrode...................... 360.1 4500-O G................ D888-92(B).................. I-1576-78\8\
47. Palladium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration, or....... 253.1 3111 B.................. ............................ ........................ p. S27.\10\
AA furnace..................... 253.2 ........................ ............................ ........................ p. S28.\10\
DCP............................ ........... ........................ ............................ ........................ Note 34.
48. Phenols, mg/L:
Manual distillation\26\........ 420.1 ........................ ............................ ........................ Note 27.
Followed by:
Colorimetric (4AAP) manual, 420.1 ........................ ............................ ........................ Note 27.
or
Automated\19\.............. 420.2
49. Phosphorus (elemental), mg/L:
Gas-liquid chromatography...... ........... ........................ ............................ ........................ Note 28.
50. Phosphorus--Total, mg/L:
Persulfate digestion followed 365.2 4500-P B,5.............. ............................ ........................ 973.55.\3\
by.
Manual or...................... 365.2 or 4500-P E................ D515-88(A)
365.3
Automated ascorbic acid 365.1 4500-P F................ ............................ I-4600-85............... 973.56.\3\
reduction.
Semi-automated block digestor.. 365.4 ........................ D515-88(B)
51. Platinum--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration............. 255.1 3111 B
AA furnace..................... 255.2
DCP............................ ........... ........................ ............................ ........................ Note 34.
52. Potassium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 258.1 3111 B.................. ............................ I-3630-85............... 973.53.\3\
ICP/AES........................ \5\200.7 3120 B
Flame photometric, or.......... ........... 3500-K D
Colorimetric................... ........... ........................ ............................ ........................ 317 B.\17\
53. Residue--Total, mg/L:
Gravimetric, 103-105 deg....... 160.3 2540 B.................. ............................ I-3750-85
54. Residue--filterable, mg/L:
Gravimetric, 180 deg........... 160.1 2540 C.................. ............................ I-1750-85
55. Residue--nonfilterable (TSS),
mg/L:
Gravimetric, 103-105 deg. post 160.2 2540 D.................. ............................ I-3765-85
washing of residue.
56. Residue--settleable, mg/L:
Volumetric, (Imhoff cone), or 160.5 2540 F
gravimetric.
57. Residue--Volatile, mg/L:
Gravimetric, 550 deg........... 160.4 ........................ ............................ I-3753-85
58. Rhodium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration, or....... 265.1 3111 B
AA furnace..................... 265.2
59. Ruthenium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration, or....... 267.1 3111 B
AA furnace..................... 267.2
60. Selenium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA furnace..................... 270.2 3113 B.................. D3859-93(B)
[[Page 17166]]
ICP/AES,\36\ or................ \5\200.7 3120 B
AA gaseous hydride............. ........... 3114 B.................. D3859-93(A)................. I-3667-85
61. Silica\37\--Dissolved, mg/L;
0.45 micron filtration followed
by:
Colorimetric, Manual or........ 370.1 4500-Si D............... D859-88..................... I-1700-85
Automated (Molybdosilicate), or ........... ........................ ............................ I-2700-85
ICP............................ \5\200.7 3120 B
62. Silver--Total,\4\ mg/L;
Digestion4,29 followed by:
AA direct aspiration........... 272.1 3111 B or C............. ............................ I-3720-85............... 974.27,\3\ p. 37.\9\
AA furnace..................... 272.2 3113 B
ICP/AES........................ \5\200.7 3120 B
DCP............................ ........... ........................ ............................ ........................ Note 34.
63. Sodium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 273.1 3111 B.................. ............................ I-3735-85............... 973.54.\3\
ICP/AES........................ \5\200.7 3120 B
DCP, or....................... ........... ........................ ............................ ........................ Note 34.
Flame photometric.............. ........... 3500 Na D
64. Specific conductance, micromhos/
cm at 25 deg.C:
Wheatstone bridge.............. 120.1 2510 B.................. D1125-91(A)................. I-1780-85............... 973.40.\3\
65. Sulfate (as SO4), mg/L:
Automated colorimetric (barium 375.1
chloranilate).
Gravimetric.................... 375.3 4500-SO4-2 C or D....... ............................ ........................ 925.54.\3\
Turbidimetric, or.............. 375.4 ........................ D516-90..................... ........................ 426C.\30\
66. Sulfide (as S), mg/L:
Titrimetric (iodine), or....... 376.1 4500-S-2 E.............. ............................ I-3840-85
Colorimetric (methylene blue).. 376.2 4500-S-2 D
67. Sulfite (as SO3), mg/L:
Titrimetric (iodine-iodate).... 377.1 4500-SO3-2 B
68. Surfactants, mg/L:
Colorimetric (methylene blue).. 425.1 5540 C.................. D2330-88
69. Temperature, deg.C:
Thermometric................... 170.1 2550 B.................. ............................ ........................ Note 32.
70. Thallium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 279.1 3111 B
AA furnace..................... 279.2
ICP/AES, or.................... \5\200.7 3120 B
71. Tin--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 282.1 3111 B.................. ............................ I-3850-78\8\
AA furnace, or................. 282.2 3113 B
ICP/AES........................ \5\200.7
72. Titanium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 283.1 3111 D
AA furnace..................... 283.2
DCP............................ ........... ........................ ............................ ........................ Note 34.
73. Turbidity, NTU:
Nephelometric.................. 180.1 2130 B.................. D1889-88(A)................. I-3860-85
74. Vanadium--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration........... 286.1 3111 D
AA furnace..................... 286.2 ........................ D3373-93
ICP/AES........................ \5\200.7 3120 B
DCP, or........................ ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Gallic acid)..... ........... 3500-V D
75. Zinc--Total,\4\ mg/L;
Digestion\4\ followed by:
AA direct aspiration\36\....... 289.1 3111 B or C............. D1691-90 (A or B)........... I-3900-85............... 974.27,\3\ p. 37.\9\
AA furnace..................... 289.2
ICP/AES\36\.................... \5\200.7 3120 B
DCP,\36\ or.................... ........... ........................ D4190-82(88)................ ........................ Note 34.
Colorimetric (Dithizone) or.... ........... 3500-Zn E
(Zincon)....................... ........... 3500-Zn F............... ............................ ........................ Note 33.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IB Notes:
[[Page 17167]]
\1\``Methods for Chemical Analysis of Water and Wastes'', Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-
CI), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.
\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, Denver, CO, Revised 1989, unless otherwise stated.
\3\``Official Methods of Analysis of the Association of Official Analytical Chemists,'' methods manual, 15th ed. (1990).
\4\For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended
material and to destroy possible organic-metal complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes,
1979 and 1983''. One (section 4.1.3), is a vigorous digestion using nitric acid. A less vigorous digestion using nitric and hydrochloric acids
(section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types. Particularly,
if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive
state. In those situations, the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing
large amounts of organic materials may also benefit by this vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert
antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as well as determinations for certain elements such as
antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all cases the
method write-up should be consulted for specific instructions and/or cautions.
Note to Table IB Note 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the
above, the EPA procedure must be used.
Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the
referenced procedure for total metals must be followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample
solution for total metals) may be omitted for AA (direct aspiration or graphite furnace) and ICP analyses, provided the sample solution to be analyzed
meets the following criteria:
a. has a low COD (<20)
b. is visibly transparent with a turbidity measurement of 1 NTU or less
c. is colorless with no perceptible odor, and
d. is of one liquid phase and free of particulate or suspended matter following acidification.
\5\The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,'' is
given at Appendix C of this Part 136.
\6\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.
\7\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.
\8\The approved method is that cited in ``Methods for Determination of Inorganic Substances in Water and Fluvial Sediments'', USGS TWRI, Book 5, Chapter
A1 (1979).
\9\American National Standard on Photographic Processing Effluents, Apr. 2, 1975. Available from ANSI, 1430 Broadway, New York, NY 10018.
\10\``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency'', Supplement to the Fifteenth Edition of
Standard Methods for the Examination of Water and Wastewater (1981).
\11\The use of normal and differential pulse voltage ramps to increase sensitivity and resolution is acceptable.
\12\Carbonaceous biochemical oxygen demand (CBOD5) must not be confused with the traditional BOD5 test 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.
\13\OIC Chemical Oxygen Demand Method, Oceanography International Corporation, 1978, 512 West Loop, P.O. Box 2980, College Station, TX 77840.
\14\Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\15\The back titration method will be used to resolve controversy.
\16\Orion Research Instruction Manual, Residual Chlorine Electrode Model 97-70, 1977, Orion Research Incorporated, 840 Memorial Drive, Cambridge, MA
02138. The calibration graph for the Orion residual chlorine method must be derived using a reagent blank and three standard solutions, containing
0.2, 1.0, and 5.0 ml 0.00281 N potassium iodate/100 ml solution, respectively.
\17\The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 14th Edition, 1976.
\18\National Council of the Paper Industry for Air and Stream Improvement, (Inc.) Technical Bulletin 253, December 1971.
\19\Copper, Biocinchoinate Method, Method 8506, Hach Handbook of Water Analysis, 1979, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\20\After the manual distillation is completed, the autoanalyzer manifolds in EPA Methods 335.3 (cyanide) or 420.2 (phenols) are simplified by
connecting the re-sample line directly to the sampler. When using the mainfold setup shown in Method 335.3, the buffer 6.2 should be replaced with the
buffer 7.6 found in Method 335.2.
\21\Hydrogen ion (pH) Automated Electrode Method, Industrial Method Number 378-75WA, October 1976, Bran & Luebbe (Technicon) Autoanalyzer II. Bran &
Luebbe Analyzing Technologies, Inc., Elmsford, NY 10523.
\22\Iron, 1,10-Phenanthroline Method, Method 8008, 1980, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\23\Manganese, Periodate Oxidation Method, Method 8034, Hach Handbook of Wastewater Analysis, 1979, pages 2-113 and 2-117, Hach Chemical Company,
Loveland, CO 80537.
\24\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.
\25\Nitrogen, Nitrite, Method 8507, Hach Chemical Company, P.O. Box 389, Loveland, CO 80537.
\26\Just prior to distillation, adjust the sulfuric-acid-preserved sample to pH 4 with 1 + 9 NaOH.
\27\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 spectophotometric procedure.
\28\R. F. Addison and R.G. Ackman, ``Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,'' Journal of Chromatography, vol. 47,
No. 3, pp. 421-426, 1970.
\29\Approved methods for the analysis of silver in industrial wastewaters at concentrations of 1 mg/L and above are inadequate where silver exists as an
inorganic halide. Silver halides such as the bromide and chloride are relatively insoluble in reagents such as nitric acid but are readily soluble in
an aqueous buffer of sodium thiosulfate and sodium hydroxide to pH of 12. Therefore, for levels of silver above 1 mg/L, 20 mL of sample should be
diluted to 100 mL by adding 40 mL each of 2 M Na2S2O3 and NaOH. Standards should be prepared in the same manner. For levels of silver below 1 mg/L the
approved method is satisfactory.
\30\The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition.
\31\EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of
total cyanide.
\32\Stevens, H.H., Ficke, J.F., and Smoot, G.F., ``Water Temperature--Influential Factors, Field Measurement and Data Presentation'', Techniques of
Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1, 1975.
\33\Zinc, Zincon Method, Method 8009, Hach Handbook of Water Analysis, 1979, pages 2-231 and 2-333, Hach Chemical Company, Loveland, CO 80537.
\34\``Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes, Method AES0029,'' 1986--
Revised 1991, Fison Instruments, Inc., 32 Commerce Center, Cherry Hill Drive, Danvers, MA 01923.
\35\Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC
method for arsenic are provided in Appendix D of this part titled, ``Precision and Recovery Statements for Methods for Measuring Metals''.
[[Page 17168]]
\36\``Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals'', CEM Corporation, P.O. Box 200, Matthews, NC 28106-0200,
April 16, 1992. Available from the CEM Corporation.
\37\When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis.
\38\Only the trichlorofluoromethane extraction solvent is approved.
Table IC.--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
--------------------------------------------------------------------------------------------------------------------------------------------------------
* * * * * * *
33. Dibenzo(a,h)anthracene...... 610................. 625, 1625........... 610 6410 B, 6440 B................ D4657-92........
* * * * * * *
37. 1,4-Dichlorobenzene......... 601, 602, 612....... 624, 625, 1625...... ......... 6410 B, 6220 B, 6230 B........
* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC 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.
\3\``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September, 1978.
* * * * * * *
5a625, Screening only.
* * * * * * *
\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 each in section 8.2 of each of these Methods. Additionally, each
laboratory, on an on-going basis must spike and analyze 10% (5% for Methods 624 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.
Table ID.--List of Approved Test Procedures for Pesticides\1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter Method EPA2,7 18th ed. ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
* * * * * * *
8.-BHC.............. GC...................... 608 6630 B & C.......... D3086-90 Note 3, p. 7.
GC/MS................... \5\625 6410 B..............
9. -BHC............. GC...................... 608 6630................ D3086-90 ........................................
GC/MS................... \5\625 6410 B..............
10. -BHC............ GC...................... 608 6630 B & C.......... D3086-90
GC/MS................... \5\625 6410 B..............
* * * * * * *
22. Demeton-S................ GC...................... ......... .................... .................... Note 3, p. 25: Note 6, p. S51.
* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID Notes:
\1\Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, where
entries are listed by chemical name.
\2\The full text of Methods 608 and 625 are given at Appendix A. ``Test Procedures for Analysis of Organic Pollutants,'' of this Part 136. The
standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B. ``Definition
and Procedure for the Determination of the Method Detection Limit'', of this Part 136.
\3\``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September, 1978. This EPA publication includes thin-layer chromatography (TLC) methods.
* * * * * * *
\5\The method may be extended to include -BHC, -BHC, endosulfan I, endosulfan II, and endrin. However, when they are known to exist,
Method 608 is the preferred method.
\6\``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency.'' Supplement to the Fifteenth Edition of
Standard Methods for the Examination of Water and Wastewater (1981).
\7\Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625
(See Appendix A of this Part 136) in accordance with procedures given in section 8.2 of each of these methods. Additionally, each laboratory, on an on-
going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate
laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits,
the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory compliance. These
quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
[[Page 17169]] * * * * *
(b) * * *
References, Sources, Costs, and Table Citations
* * * * *
(10) Annual Book of ASTM Standards, Water and Environmental
Technology, Section 11, Volumes 11.01 and 11.02, 1994 in 40 CFR 136.3,
Tables IB, IC, ID and IE.
* * * * *
(e) * * *
Table II.--Required Containers, Preservation Techniques, and Holding Times
--------------------------------------------------------------------------------------------------------------------------------------------------------
Maximum
Parameter Container\1\ Preservation\2\\3\ holding
time\4\
--------------------------------------------------------------------------------------------------------------------------------------------------------
* * * * * * *
Table IB--Inorganic Tests:
* * * * * * *
10. Boron............................ P, PFTE, or Quartz.............. HNO3 to pH<2................................................ 6 months.
* * * * * * *
Metals\7\
* * * * * * *
3, 5-8, 12, 13, 19, 20, 22, 26, 29, P, G............................ HNO3 to pH<2................................................ 6 months.
30, 32-34, 36, 37, 45, 47, 51, 52,
58-60, 62, 63, 70-72, 74, 75.
Metals, except boron, chromium VI
and mercury.
* * * * * * *
42. Organic Carbon....................... P, G............................ Cool to 4 deg.C, HCl or H22SO4 or H3PO4, to pH<2............ 28 days.
* * * * * * *
61. Silica............................... P, PFTE, or Quartz.............. Cool, 4 deg.C............................................... 28 days.
* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table II--Notes:
\1\Polyethylene (P) or Glass (G).
\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\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).
\4\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.
* * * * * * *
\7\Samples should be filtered immediately on-site before adding preservative for dissolved metals.
* * * * * * *
[FR Doc. 95-5022 Filed 4-3-95; 8:45 am]
BILLING CODE 6560-50-P