17160 Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations

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,
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations 17161

except boron, chromium VI and

mercury’’, 42 and 61, to read as follows:

§ 136.3 Identification of test procedures.

(a) * * *

TABLE IA.—LIST OF APPROVED BIOLOGICAL TEST PROCEDURES

Parameter, units and method Method 1

Reference (method No. or page)

EPA2

Standard

methods 18th

ed.

ASTM USGS3

Bacteria:

1. Coliform (fecal), number per 100 mL ......... Most Probable Number (MPN), 5

tube, 3 dilution.

p. 132 ..... 9221C and E.

Membrane filter (MF)4, single

step.

p. 124 ..... 9222D B–0050–

85

2. Coliform (fecal) in presence of chlorine,

number per 100 mL.

MPN, 5 tube, 3 dilution ...............

MF4, single step 5 ........................

p. 132 .....

p. 124 .....

9221C and E .

9222D

* * * * * * *

Table IA Notes:

1The method used must be specified when results are reported.

2Bordner, 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. 3Britton, 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. 4A 0.45 μm membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated, and to be free of

extractables which could interfere with their growth. 5Because 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

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

1. Acidity, as CaCO3, mg/L:

Electrometric endpoint or phenolphthalein endpoint.305.1 2310 B(4a) ............. D1067–92

2. Alkalinity, as CaCO3, mg/L:

Electrometric or Colorimetric titration to pH 4.5, manual or automated.310.1

310.2

2320 B ....................

................................

D1067–92 .....................

.......................................

I–1030–85 ..............

I–2030–85

973.43.3

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/Atomic Emission Spectrometry (ICP/

AES) 36.

5 200.7 3120 B

Direct Current Plasma (DCP) 36 .... ................... ................................ D4190–82(88) .............. ................................ Note 34.

Colorimetric (Eriochrome cyanine

R).

................... 3500–Al D

4. Ammonia (as N), mg/L:

Manual, distillation (at pH 9.5),6

followed by.

350.2 4500–NH3 B ........... ....................................... ................................ 973.49.3

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/AES36 .................................... 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)
17162 Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations

TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

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/AES36 .................................... 5 200.7 3120 B

DCP36 ........................................... ................... ................................ ....................................... ................................ 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/AES36 .................................... 5 200.7 3120 B .................... ....................................... I–1472–85

DCP36 ........................................... ................... ................................ 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

nitrification inhibitor.

................... 5210 B

15. Chemical oxygen demand (COD),

mg/L; Titrimetric, or.

410.1

410.2

410.3

5220 C ...................

................................

D1252–88(A) ................

.......................................

I–3560–85 ..............

I–3562–85 ..............

973.46,3 p. 17.9

Spectrophotometric, manual or

automated.

410.4 5220 D ................... D1252–88(B) ................ I–3561–85 .............. Notes 13 or 14.

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

325.2

4500–Cl¥ E ........... ....................................... I–2187–85

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- point 15 or 330.2 4500–Cl C

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 (Diphenylcarbazide) .. ................... 3500–Cr D .............. D1687–92(A) ................ I–1230–85

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
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations 17163

TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

AA chelation-extraction ................. 218.3 3111 C

AA furnace .................................... 218.2 3113 B .................... D1687–92(C)

ICP/AES36 .................................... 5 200.7 3120 B

DCP,36 or ...................................... ................... ................................ D4190–82(88) .............. ................................ Note 34.

Colorimetric (Diphenylcarbazide) ................... 3500–Cr D

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; Digestion 4

followed by:

AA direct aspiration 36 ................... 220.1 3111 B or C ........... D1688–90(A or B) ........ I–3270–85 or

I3271–85.

974.27 3 p. 37.9

AA furnace .................................... 220.2 3113 B .................... D1688–90(C)

ICP/AES36 ..................................... 5 200.7 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 followed by.................... 4500–CN C ............ D2036–91(A)

Titrimetric, or ................................. ................... 4500–CN D ............ ....................................... ................................ p. 22.9

Spectrophotometric, manual or ..... 31 335.2 4500–CN E ............ D2036–91(A) ................ I–3300–85

Automated 20 ................................. 31 335.3

24. Cyanide amenable to

chlorination,mg/L:

Manual distillation with MgCl2 followed by titrimetric or

Spectrophotometric.

335.1 4500–CN G ............ D2036–91(B)

25. Fluoride—Total, mg/L:

Manual distillation 6 followed by .... ................... 4500–F B

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; Digestion 4 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 Mg

as their carbonates, by inductively coupled plasma or AA direct aspiration. (See Parameters

13 and 33).

130.2 2340 B or C ........... D1126–86(92) .............. I–1338–85 .............. 973.52B.3

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; Digestion 4

followed by:

AA direct aspiration or .................. 235.1 3111 B

AA furnace .................................... 235.2

30. Iron—Total,4 mg/L; Digestion 4 followed by:

AA direct aspiration 36 ................... 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 ..................................... 5 200.7 3120 B

DCP36 or ....................................... ................... ................................ D4190–82(88) .............. ................................ Note 34.

Colorimetric (Phenanthroline) ....... ................... 3500–Fe D ............. D1068–90(D) ................ ................................ Note 22.
17164 Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations

TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

31. Kjeldahl Nitrogen—Total, (as N),

mg/L

Digestion and distillation followed

by.

351.3 4500–NH3 B or C ... D3590–89(A)

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–4551–78 8

Semi-automated block digestor

colorimetric, or.

351.2 ................................ D3590–89(B)

Manual or block digestor

Potentiometric.

351.4 ................................ D3590–89(A)

32. Lead—Total,4 mg/L; Digestion 4 followed by:

AA direct aspiration 36 ................... 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 ..................................... 5 200.7 3120 B

DCP36 ........................................... ................... ................................ D4190–82(88) .............. ................................ Note 34.

Voltametry 11 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/AES36 .................................... 5 200.7 3120 B

DCP36 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/AES36 .................................... 5 200.7 3120 B

DCP36, or ...................................... ................... ................................ D4190–82(88) .............. ................................ Note 34.

Colorimetric (heptoxime) ............... ................... 3500–Ni D

38. Nitrate (as N), mg/L:

Colorimetric (Brucine sulfate), or

Nitrate-nitrite N minus Nitrite N

(See parameters 39 and 40).

352.1 ................................ ....................................... ................................ 973.50,3 419

D,17 p. 28.9

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 B38

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:
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations 17165

TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

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), or .... 360.2 4500–O C ............... D888–92(A) .................. I–1575–78 8 ............ 973.45B.3

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,

or

420.1 ................................ ....................................... ................................ Note 27.

Automated 19 .......................... 420.2

49. Phosphorus (elemental), mg/L:

Gas-liquid chromatography ........... ................... ................................ ....................................... ................................ Note 28.

50. Phosphorus—Total, mg/L:

Persulfate digestion followed by ... 365.2 4500–P B,5 ............ ....................................... ................................ 973.55.3

Manual or ...................................... 365.2 or

365.3

4500–P E ............... D515–88(A)

Automated ascorbic acid reduction 365.1 4500–P F ............... ....................................... I–4600–85 .............. 973.56.3

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° .................. 160.3 2540 B .................... ....................................... I–3750–85

54. Residue—filterable, mg/L:

Gravimetric, 180° .......................... 160.1 2540 C ................... ....................................... I–1750–85

55. Residue—nonfilterable (TSS), mg/

L:

Gravimetric, 103–105° post washing of residue.160.2 2540 D ................... ....................................... I–3765–85

56. Residue—settleable, mg/L:

Volumetric, (Imhoff cone), or

gravimetric.

160.5 2540 F

57. Residue—Volatile, mg/L:

Gravimetric, 550° .......................... 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)
17166 Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations

TABLE IB.—LIST OF APPROVED INORGANIC TEST PROCEDURES—Continued

Parameter, units and method

Reference (method number or page)

EPA1,35 STD methods

18th ed. ASTM USGS2 Other

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; Digestion 4, 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 °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

chloranilate).

375.1

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, °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/AES36 .................................... 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:
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations 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. 2Fishman, 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).

4For 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. 5The 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. 7Ammonia, 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. 8The approved method is that cited in ‘‘Methods for Determination of Inorganic Substances in Water and Fluvial Sediments’’, USGS TWRI,

Book 5, Chapter A1 (1979). 9American 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). 11The 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. 13OIC 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. 15The back titration method will be used to resolve controversy. 16Orion 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. 17The 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. 20After 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. 24Wershaw, 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. 27The 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 10.0±0.2. 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. 29Approved 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. 30The approved method is that cited in Standard Methods for the Examination of Water and Wastewater, 15th Edition. 31EPA 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. 32Stevens, 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. 33Zinc, 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. 35Precision 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’’.
17168 Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations

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. 37When determining boron and silica, only plastic, PTFE, or quartz laboratory ware may be used from start until completion of analysis. 38Only the trichlorofluoromethane extraction solvent is approved.

TABLE IC.—LIST OF APPROVED TEST PROCEDURES FOR NON-PESTICIDE ORGANIC COMPOUNDS

Parameter 1

EPA method number 2, 7 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:

1All parameters are expressed in micrograms per liter (μg/L). 2The 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.

* * * * * * *

5a 625, Screening only.

* * * * * * *

7Each 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 PESTICIDES1

Parameter Method EPA2, 7 Standard methods 18th ed. ASTM Other

* * * * * * *

8.α-BHC ........................................... GC .........................

GC/MS ...................

608

5 625

6630 B & C .......

6410 B ..............

D3086–90 Note 3, p. 7.

9. β-BHC .......................................... GC .........................

GC/MS ...................

608

5 625

6630 .................

6410 B ..............

D3086–90

10. δ-BHC ........................................ GC .........................

GC/MS ...................

608

5 625

6630 B & C .......

6410 B ..............

D3086–90

* * * * * * *

22. Demeton-S ................................ GC ......................... ............... ........................... Note 3, p. 25: Note 6, p. S51.

* * * * * * *

Table ID Notes:

1Pesticides 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. 2The 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.

* * * * * * *

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

Method 608 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). 7Each 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.
Federal Register / Vol. 60, No. 64 / Tuesday, April 4, 1995 / Rules and Regulations 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

Parameter Container 1 Preservation 2 3

Maximum

holding

time 4

* * * * * * *

Table IB—Inorganic Tests:

* * * * * * *

10. Boron ........................................................ P, PFTE, or Quartz ........... HNO 3 to pH<2 ....................................................... 6 months.

* * * * * * *

Metals 7

* * * * * * *

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, except boron, chromium VI and mercury.

P, G .................................. HNO3 to pH<2 ........................................................ 6 months.

* * * * * * *

42. Organic Carbon ............................................... P, G .................................. Cool to 4°C, HCl or H22SO4 or H3PO4, to pH<2 .. 28 days.

* * * * * * *

61. Silica ................................................................ P, PFTE, or Quartz .......... Cool, 4°C ................................................................ 28 days.

* * * * * * *

Table II—Notes:

1Polyethylene (P) or Glass (G).

2Sample 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°C until compositing and sample splitting is completed. 3When 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). 4Samples 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 § 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 § 136.3(e) for details. The term ‘‘analyze immediately’’ usually means within 15 minutes or less of sample collection.

* * * * * * *

7Samples 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