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(continued)
toluene........................ 108-88-3........................... D3695/D4763/502.2/524.2.
triethlyamine.................. 121-44-8........................... 1666/1671.
xylenes........................ (Note 1)........................... 1624C/1666.
----------------------------------------------------------------------------------------------------------------
Table 1F note:
1. 1624C: m-xylene 108-38-3, o,p-xylene E-14095 (Not a CAS number; this is the number provided in the
Environmental Monitoring Methods Index (EMMI) database.); 1666: m,p-xylene 136777-61-2, o-xylene 95-47-6.


(b) The full texts of the methods from the following references which are cited in Tables IA, IB, IC, ID, IE,and IF are incorporated by reference into this regulation and may be obtained from the sources identified. All costs cited are subject to change and must be verified from the indicated sources. The full texts of all the test procedures cited are available for inspection at the National Exposure Research Laboratory, Office of Research and Development, U.S. Environmental Protection Agency, 26 West Martin Luther King Dr., Cincinnati, OH 45268 and the National Archives and Records Administration (NARA). For information on the availability of this material at NARA, call 202–741–6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.

References, Sources, Costs, and Table Citations:

(1) The full texts of Methods 601–613, 624, 625, 1613, 1624, and 1625 are printed in appendix A of this part 136. The full text for determining the method detection limit when using the test procedures is given in appendix B of this part 136. The full text of Method 200.7 is printed in appendix C of this part 136. Cited in: Table IB, Note 5; Table IC, Note 2; and Table ID, Note 2.

(2) USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. EPA/600/8–78/017. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Publ. No. PB–290329/AS. Cost: $36.95. Table IA, Note 3.

(3) “Methods for Chemical Analysis of Water and Wastes,” U.S. Environmental Protection Agency, EPA–600/4–79–020, March 1979, or “Methods for Chemical Analysis of Water and Wastes,” U.S. Environmental Protection Agency, EPA–600/4–79–020, Revised March 1983. Available from: ORD Publications, CERI, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268, Table IB, Note 1.

(4) “Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,” U.S. Environmental Protection Agency, 1978. Available from: ORD Publications, CERI, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268, Table IC, Note 3; Table D, Note 3.

(5) “Prescribed Procedures for Measurement of Radioactivity in Drinking Water,” U.S. Environmental Protection Agency, EPA–600/4–80–032, 1980. Available from: ORD Publications, CERI, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268, Table IE, Note 1.

(6) American Public Health Association. 1992, 1995, and 1998. Standard Methods for the Examination of Water and Wastewater. 18th, 19th, and 20th Edition (respectively). Available from: Amer. Publ. Hlth. Assoc., 1015 15th Street, NW., Washington, DC 20005. Table IA, Note 4. Tables IB, IC, ID, IE.

(7) Ibid, 15th Edition, 1980. Table IB, Note 30; Table ID.

(8) Ibid, 14th Edition, 1975. Table IB, Notes 17 and 27.

(9) “Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency,” Supplement to the 15th Edition of Standard Methods for the Examination of Water and Wastewater, 1981. Available from: American Public Health Association, 1015 Fifteenth Street NW., Washington, DC 20036. Cost available from publisher. Table IB, Note 10; Table IC, Note 6; Table ID, Note 6.

(10) Annual Book of ASTM Standards, Water, and Environmental Technology, Section 11, Volumes 11.01 and 11.02, 1994, 1996, 1999, and Volume 11.02, 2000 in 40 CFR 136.3, Tables IA, IB, IC, ID, and IE.

(11) USGS. 1989. U.S. Geological Survey Techniques of Water-Resources Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of the Interior, Reston, Virginia. Available from: USGS Books and Open-File Reports Section, Federal Center, Box 25425, Denver, Colorado 80225. Cost: $18.00. Table IA, Note 5.

(12) “Methods for Determination of Inorganic Substances in Water and Fluvial Sediments,” by M.J. Fishman and Linda C. Friedman, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5 Chapter A1 (1989). Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $108.75 (subject to change). Table IB, Note 2.

(13) “Methods for Determination of Inorganic Substances in Water and Fluvial Sediments,” N.W. Skougstad and others, editors. Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A1 (1979). Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $10.00 (subject to change), Table IB, Note 8.

(14) “Methods for the Determination of Organic Substances in Water and Fluvial Sediments,” Wershaw, R.L., et al, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter A3 (1987). Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $0.90 (subject to change). Table IB, Note 24; Table ID, Note 4.

(15) “Water Temperature—Influential Factors, Field Measurement and Data Presentation,” by H.H. Stevens, Jr., J. Ficke, and G.F. Smoot, Techniques of Water-Resources Investigations of the U.S. Geological Survey, Book 1, Chapter D1, 1975. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Cost: $1.60 (subject to change). Table IB, Note 32.

(16) “Selected Methods of the U.S. Geological Survey of Analysis of Wastewaters,” by M.J. Fishman and Eugene Brown; U.S. Geological Survey Open File Report 76–77 (1976). Available from: U.S. Geological Survey, Branch of Distribution, 1200 South Eads Street, Arlington, VA 22202. Cost: $13.50 (subject to change). Table IE, Note 2.

(17) “Official Methods of Analysis of the Association of Official Analytical Chemicals”, Methods manual, 15th Edition (1990). Price: $240.00. Available from: The Association of Official Analytical Chemists, 2200 Wilson Boulevard, Suite 400, Arlington, VA 22201. Table IB, Note 3.

(18) “American National Standard on Photographic Processing Effluents,” April 2, 1975. Available from: American National Standards Institute, 1430 Broadway, New York, New York 10018. Table IB, Note 9.

(19) “An Investigation of Improved Procedures for Measurement of Mill Effluent and Receiving Water Color,” NCASI Technical Bulletin No. 253, December 1971. Available from: National Council of the Paper Industry for Air and Stream Improvements, Inc., 260 Madison Avenue, New York, NY 10016. Cost available from publisher. Table IB, Note 18.

(20) Ammonia, Automated Electrode Method, Industrial Method Number 379–75WE, dated February 19, 1976. Technicon Auto Analyzer II. Method and price available from Technicon Industrial Systems, Tarrytown, New York 10591. Table IB, Note 7.

(21) Chemical Oxygen Demand, Method 8000, Hach Handbook of Water Analysis, 1979. Method price available from Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 14.

(22) OIC Chemical Oxygen Demand Method, 1978. Method and price available from Oceanography International Corporation, 512 West Loop, P.O. Box 2980, College Station, Texas 77840. Table IB, Note 13.

(23) ORION Research Instruction Manual, Residual Chlorine Electrode Model 97–70, 1977. Method and price available from ORION Research Incorporation, 840 Memorial Drive, Cambridge, Massachusetts 02138. Table IB, Note 16.

(24) Bicinchoninate Method for Copper. Method 8506, Hach Handbook of Water Analysis, 1979, Method and price available from Hach Chemical Company, P.O. Box 300, Loveland, Colorado 80537. Table IB, Note 19.

(25) Hydrogen Ion (pH) Automated Electrode Method, Industrial Method Number 378–75WA. October 1976. Bran & Luebbe (Technicon) Auto Analyzer II. Method and price available from Bran & Luebbe Analyzing Technologies, Inc. Elmsford, N.Y. 10523. Table IB, Note 21.

(26) 1,10-Phenanthroline Method using FerroVer Iron Reagent for Water, Hach Method 8008, 1980. Method and price available from Hach Chemical Company, P.O. Box 389 Loveland, Colorado 80537. Table IB, Note 22.

(27) Periodate Oxidation Method for Manganese, Method 8034, Hach Handbook for Water Analysis, 1979. Method and price available from Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 23.

(28) Nitrogen, Nitrite—Low Range, Diazotization Method for Water and Wastewater, Hach Method 8507, 1979. Method and price available from Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 25.

(29) Zincon Method for Zinc, Method 8009. Hach Handbook for Water Analysis, 1979. Method and price available from Hach Chemical Company, P.O. Box 389, Loveland, Colorado 80537. Table IB, Note 33.

(30) “Direct Determination of Elemental Phosphorus by Gas-Liquid Chromatography,” by R.F. Addison and R.G. Ackman, Journal of Chromatography, Volume 47, No. 3, pp. 421–426, 1970. Available in most public libraries. Back volumes of the Journal of Chromatography are available from Elsevier/North-Holland, Inc., Journal Information Centre, 52 Vanderbilt Avenue, New York, NY 10164. Cost available from publisher. Table IB, Note 28.

(31) “Direct Current Plasma (DCP) Optical Emission Spectrometric Method for Trace Elemental Analysis of Water and Wastes”, Method AES 0029, 1986-Revised 1991, Fison Instruments, Inc., 32 Commerce Center, Cherry Hill Drive, Danvers, MA 01923. Table B, Note 34.

(32) “Closed Vessel Microwave Digestion of Wastewater Samples for Determination of Metals, CEM Corporation, P.O. Box 200, Matthews, North Carolina 28106–0200, April 16, 1992. Available from the CEM Corporation. Table IB, Note 36.

(33) “Organochlorine Pesticides and PCBs in Wastewater Using EmporeTM Disk” Test Method 3M 0222, Revised 10/28/94. 3M Corporation, 3M Center Building 220–9E–10, St. Paul, MN 55144–1000. Method available from 3M Corporation. Table IC, Note 8 and Table ID, Note 8.

(34) USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA 821–R–02–012. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002–108488. Table IA, Note 29.

(35) “Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection)”, revised 12/22/94. Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd., Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 39.

(36) “Nitrogen, Total Kjeldahl, Method PAI-DK02 (Block Digestion, Steam Distillation, Colorimetric Detection)”, revised 12/22/94. Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd., Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 40.

(37) “Nitrogen, Total Kjeldahl, Method PAI-DK03 (Block Digestion, Automated FIA Gas Diffusion)”, revised 12/22/94. Available from Perstorp Analytical Corporation, 9445 SW Ridder Rd., Suite 310, P.O. Box 648, Wilsonville, OK 97070. Table IB, Note 41.

(38) USEPA. October 2002. Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–02–013. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002–108489. Table IA, Note 30.

(39) USEPA. October 2002. Short-Term Methods for Measuring the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA–821–R–02–014. Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161, Pub. No. PB2002–108490. Table IA, Note 31.

(40) EPA Methods 1666, 1667, and 1671 listed in the table above are published in the compendium titled Analytical Methods for the Determination of Pollutants in Pharmaceutical Manufacturing Industry Wastewaters (EPA 821–B–98–016). EPA Methods 502.2 and 524.2 have been incorporated by reference into 40 CFR 141.24 and are in Methods for the Determination of Organic Compounds in Drinking Water, EPA–600/4–88–039, December 1988, Revised, July 1991, and Methods for the Determination of Organic Compounds in Drinking Water-Supplement II, EPA–600/R–92–129, August 1992, respectively. These EPA test method compendia are available from the National Technical Information Service, NTIS PB91–231480 and PB92–207703, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161. The toll-free number is 800–553–6847. ASTM test methods D3371, D3695, and D4763 are available from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428–2959.

(41) USEPA. 2002. Method 1631, Revision E, “Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry.” September 2002. Office of Water, U.S. Environmental Protection Agency (EPA–821–R–02–019). Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161. Publication No. PB2002–108220. Cost: $25.50 (subject to change).

(42) [Reserved]

(43) Method OIA–1677, Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry. August 1999. ALPKEM, OI Analytical, Box 648, Wilsonville, Oregon 97070 (EPA–821–R–99–013). Available from: National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia 22161. Publication No. PB99–132011. Cost: $22.50. Table IB, Note 44.

(44) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory Determination of Ammonium Plus Organic Nitrogen by a Kjeldahl Digestion Method and an Automated Photometric Finish that Includes Digest Cleanup by Gas Diffusion”, Open File Report (OFR) 00–170. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 45.

(45) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Chromium in Water by Graphite Furnace Atomic Absorption Spectrophotometry”, Open File Report (OFR) 93–449. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 46.

(46) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Molybdenum in Water by Graphite Furnace Atomic Absorption Spectrophotometry”, Open File Report (OFR) 97–198. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 47.

(47) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Total Phosphorus by Kjeldahl Digestion Method and an Automated Colorimetric Finish That Includes Dialysis” Open File Report (OFR) 92–146. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 48.

(48) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Arsenic and Selenium in Water and Sediment by Graphite Furnace—Atomic Absorption Spectrometry” Open File Report (OFR) 98–639. Table IB, Note 49.

(49) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry” , Open File Report (OFR) 98–165. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 50.

(50) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Triazine and Other Nitrogen-containing Compounds by Gas Chromatography with Nitrogen Phosphorus Detectors” U.S.Geological Survey Open File Report 94–37. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table ID, Note 9.

(51) “Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediments”, Open File Report (OFR) 93–125. Available from: U.S. Geological Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 51; Table IC, Note 9.

(52) IDEXX Laboratories, Inc. 2002. Description of Colilert®, Colilert-18®”, Quanti-Tray®, Quanti-Tray®/2000, Enterolert® methods are available from IDEXX Laboratories, Inc., One Idexx Drive, Westbrook, Maine 04092. Table IA, Notes 17 and 23.

(53) Hach Company, Inc. Revision 2, 1999. Description of m-ColiBlue24® Method, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010. Table IA, Note 18.

(54) USEPA. 2002. Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar (mTEC). U.S. Environmental Protection Agency, Office of Water, Washington D.C. September 2002, EPA–821–R–02–020. Available at NTIS, PB2003–100125. Table IA, Note 20.

(55) USEPA. 2002. Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S. Environmental Protection Agency, Office of Water, Washington D.C. September 2002, EPA–821–R–02–021. Available at NTIS, PB2003–100126. Table IA, Note 24.

(56) USEPA. 2002. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli Agar (Modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC September 2002, EPA–821–R–02–023. Available at NTIS, PB2003–100128. Table IA, Note 21.

(57) Brenner et al. 1993. New Medium for the Simultaneous Detection of Total Coliforms and Escherichia coli in Water. Appl. Environ. Microbiol. 59:3534–3544. Available from the American Society for Microbiology, 1752 N Street NW., Washington, DC 20036. Table IA, Note 22.

(58) USEPA. 2002. Method 1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration using a Simultaneous Detection Technique (MI Medium). U.S. Environmental Protection Agency, Office of Water, Washington D.C. September 2002, EPA 821–R–02–024. Available from NTIS, PB2003–100129. Table IA, Note 22.

(59) USEPA. 2002. Method 1600: Enterococci in Water by Membrane Filtration using membrane-Enterococcus Indoxyl-ß-D-Glucoside Agar (mEI). U.S. Environmental Protection Agency, Office of Water, Washington D.C. September 2002, EPA–821–R–02–022. Available from NTIS, PB2003–100127. Table IA, Note 25.

(60) USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC April 2001, EPA–821–R–01–026.

Available from NTIS, PB2002–108709. Table IA, Note 26.

(61) USEPA. 2001. Method 1623: Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC April 2001, EPA–821–R–01–025. Available from NTIS, PB2002–108710. Table IA, Note 27.

(62) AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. AOAC International. 481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877–2417. Table IA, Note 11.

(c) Under certain circumstances the Regional Administrator or the Director in the Region or State where the discharge will occur may determine for a particular discharge that additional parameters or pollutants must be reported. Under such circumstances, additional test procedures for analysis of pollutants may be specified by the Regional Administrator, or the Director upon the recommendation of the Director of the Environmental Monitoring Systems Laboratory—Cincinnati.

(d) Under certain circumstances, the Administrator may approve, upon recommendation by the Director, Environmental Monitoring Systems Laboratory—Cincinnati, additional alternate test procedures for nationwide use.

(e) Sample preservation procedures, container materials, and maximum allowable holding times for parameters cited in Tables IA, IB, IC, ID, and IE are prescribed in Table II. Any person may apply for a variance from the prescribed preservation techniques, container materials, and maximum holding times applicable to samples taken from a specific discharge. Applications for variances may be made by letters to the Regional Administrator in the Region in which the discharge will occur. Sufficient data should be provided to assure such variance does not adversely affect the integrity of the sample. Such data will be forwarded, by the Regional Administrator, to the Director of the Environmental Monitoring Systems Laboratory—Cincinnati, Ohio for technical review and recommendations for action on the variance application. Upon receipt of the recommendations from the Director of the Environmental Monitoring Systems Laboratory, the Regional Administrator may grant a variance applicable to the specific charge to the applicant. A decision to approve or deny a variance will be made within 90 days of receipt of the application by the Regional Administrator.


Table II_Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
Parameter No./name Container \1\ Preservation 2,3 Maximum holding time \4\
----------------------------------------------------------------------------------------------------------------
Table IA_Bacteria Tests:
1-5 Coliform, total, fecal, PP, G........... Cool, <10 °C, 0.0008% 6 hours.
and E. coli. Na2S2O3 5.
6 Fecal streptococci.......... PP, G........... Cool, <10° 0.0008% 6 hours.
Na2S2O3 5.
7 Enterococci................. PP, G........... Cool, <10° 0.0008% 6 hours.
Na2S2O3 5.
Table IA_Protozoa Tests:
8 Cryptosporidium............. LDPE............ 0-8 °C...................... 96 hours. \17\
9 Giardia..................... LDPE............ 0-8 °C...................... 96 hours. \17\
Table IA_Aquatic Toxicity Tests:
6-10 Toxicity, acute and P,G............. Cool, 4 °C 16............... 36 hours.
chronic.

Table IB_Inorganic Tests:
1. Acidity.................... P, G............ Cool, 4°C................... 14 days.
2. Alkalinity................. P, G............ ......do........................ Do.
4. Ammonia.................... P, G............ Cool, 4°C, H2SO4 to pH<2. 28 days.
9. Biochemical oxygen demand.. P, G............ Cool, 4°C................... 48 hours.
10. Boron..................... P, PFTE, or HNO3 TO pH<2................. 6 months.
Quartz.
11. Bromide................... P, G............ None required................... 28 days.
14. Biochemical oxygen demand, P, G............ Cool, 4°C................... 48 hours.
carbonaceous.
15. Chemical oxygen demand.... P, G............ Cool, 4°C, H2SO4 to pH<2. 28 days.
16. Chloride.................. P, G............ None required................... Do.
17. Chlorine, total residual.. P, G............ ......do........................ Analyze immediately.
21. Color..................... P, G............ Cool, 4°C................... 48 hours.
23-24. Cyanide, total and P, G............ Cool, 4°C, NaOH to pH>12, 14 days. 6
amenable to chlorination. 0.6g ascorbic acid 5.
25. Fluoride.................. P............... None required................... 28 days.
27. Hardness.................. P, G............ HNO3 to pH<2, H2SO4 to 6 months.
pH<2.
28. Hydrogen ion (pH)......... P, G............ None required................... Analyze immediately.
31, 43. Kjeldahl and organic P, G............ Cool, 4°C, H2SO4 to pH<2. 28 days.
nitrogen.
Metals: 7
18. Chromium VI \7\........... P, G............ Cool, 4 °C.................. 24 hours.
35. Mercury \17\.............. P, G............ HNO3 to pH<2................. 28 days.
3, 5-8, 12,13, 19, 20, 22, 26, P, G............ do.............................. 6 months.
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 \7\.
38. Nitrate................... P, G............ Cool, 4°C................... 48 hours.
39. Nitrate-nitrite........... P, G............ Cool, 4°C, H2SO4 to pH<2. 28 days.
40. Nitrite................... P, G............ Cool, 4°C................... 48 hours.
41. Oil and grease............ G............... Cool to 4°C, HCl or H2SO4 to 28 days.
pH<2.
42. Organic Carbon............ P, G............ Cool to 4 °C HC1 or H2SO4 or 28 days.
H3PO4, to pH<2.
44. Orthophosphate............ P, G............ Filter immediately, Cool, 48 hours.
4°C.
46. Oxygen, Dissolved Probe... G Bottle and top None required................... Analyze immediately.
47. Winkler................... ......do........ Fix on site and store in dark... 8 hours.
48. Phenols................... G only.......... Cool, 4°C, H2SO4 to pH<2. 28 days.
49. Phosphorus (elemental).... G............... Cool, 4°C................... 48 hours.
50. Phosphorus, total......... P, G............ Cool, 4°C, H2SO4 to pH<2. 28 days.
53. Residue, total............ P, G............ Cool, 4°C................... 7 days.
54. Residue, Filterable....... P, G............ ......do........................ 7 days.
55. Residue, Nonfilterable P, G............ ......do........................ 7 days.
(TSS).
56. Residue, Settleable....... P, G............ ......do........................ 48 hours.
57. Residue, volatile......... P, G............ ......do........................ 7 days.
61. Silica.................... P, PFTE, or Cool, 4 °C.................. 28 days.
Quartz.
64. Specific conductance...... P, G............ ......do........................ Do.
65. Sulfate................... P, G............ ......do........................ Do.
66. Sulfide................... P, G............ Cool, 4°C add zinc acetate 7 days.
plus sodium hydroxide to
pH>9.
67. Sulfite................... P, G............ None required................... Analyze immediately.
68. Surfactants............... P ,G............ Cool, 4°C................... 48 hours.
69. Temperature............... P, G............ None required................... Analyze.
73. Turbidity................. P, G............ Cool, 4°C................... 48 hours.
Table IC_Organic Tests \8\
13, 18-20, 22, 24-28, 34-37, G, Teflon-lined Cool, 4 °C, 0.008% Na2S2O3 14 days.
39-43, 45-47, 56, 76, 104, septum. \5\..
105, 108-111, 113. Purgeable
Halocarbons.
6, 57, 106. Purgeable aromatic ......do........ Cool, 4 °C, 0.008% Na2S2O3, Do.
hydrocarbons. \5\ HCl to pH2 \9\.
3, 4. Acrolein and ......do........ Cool, 4 °C, 0.008% Na2S2O3, Do.
acrylonitrile. \5\ adjust pH to 4-5 10.
23, 30, 44, 49, 53, 77, 80, G, Teflon-lined Cool, 4 °C, 0.008% Na2S2O3 7 days until extraction;
81, 98, 100, 112. Phenols 11. cap.. \5\. 40 days after extraction.
7, 38. Benzidines 11.......... ......do........ ......do........................ 7 days until extraction.
13
14, 17, 48, 50-52. Phthalate ......do........ Cool, 4 °C.................. 7 days until extraction;
esters 11. 40 days after extraction.
82-84. Nitrosamines 11 14..... ......do........ Cool, 4 °C, 0.008% Na2S2O3, Do.
\5\ store in dark.
88-94. PCBs 11................ .....do......... Cool, 4 °C.................. Do.
54, 55, 75, 79. Nitroaromatics ......do........ Cool, 4 °C, 0.008% Na2S2O3, Do.
and isophorone 11. \5\ store in dark.
1, 2, 5, 8-12, 32, 33, 58, 59, ......do........ ......do........................ Do.
74, 78, 99, 101. Polynuclear
aromatic hydrocarbons 11.
15, 16, 21, 31, 87. Haloethers ......do........ Cool, 4 °C, 0.008% Na2S2O3 Do.
11. \5\.
29, 35-37, 63-65, 73, 107. ......do........ Cool, 4 °C.................. Do.
Chlorinated hydrocarbons 11.
60-62, 66-72, 85, 86, 95-97,
102, 103. CDDs/CDFs 11.
aqueous: field and lab G............... Cool, 0-4 °C, pH<9, 1 year.
preservation.. 0.008% Na2S2O3 \5\.
Solids, mixed phase, and ......do........ Cool, <4 °C.............. 7 days.
tissue: field preservation..
Solids, mixed phase, and ......do........ Freeze, <-10 °C.......... 1 year.
tissue: lab preservation.
Table ID_Pesticides Tests:
1-70. Pesticides \11\......... ......do........ Cool, 4°C, pH 5-9 15........ Do.
Table IE_Radiological Tests:
1-5. Alpha, beta and radium... P, G............ HNO3 to pH<2................. 6 months.
----------------------------------------------------------------------------------------------------------------
Table II Notes
\1\ Polyethylene (P) or glass (G). For microbiology, plastic sample containers must be made of sterilizable
materials (polypropylene or other autoclavable plastic).
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°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 § 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.
5 Should only be used in the presence of residual chlorine.
6 Maximum holding time is 24 hours when sulfide is present. Optionally all samples may be tested with lead
acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide is present, it can
be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample is
filtered and then NaOH is added to pH 12.
7 Samples should be filtered immediately on-site before adding preservative for dissolved metals.
8 Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
9 Sample receiving no pH adjustment must be analyzed within seven days of sampling.
10 The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
adjustment must be analyzed within 3 days of sampling.
11 When the extractable analytes of concern fall within a single chemical category, the specified preservative
and maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of
concern fall within two or more chemical categories, the sample may be preserved by cooling to 4°C,
reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9;
samples preserved in this manner may be held for seven days before extraction and for forty days after
extraction. Exceptions to this optional preservation and holding time procedure are noted in footnote 5 (re
the requirement for thiosulfate reduction of residual chlorine), and footnotes 12, 13 (re the analysis of
benzidine).
12 If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ±0.2 to prevent
rearrangement to benzidine.
13 Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)
atmosphere.
14 For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
of sampling.
15 The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still
present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, it
is necessary to immediately measure the temperature of the samples and confirm that the 4C temperature maximum
has not been exceeded. In the isolated cases where it can be documented that this holding temperature can not
be met, the permittee can be given the option of on-site testing or can request a variance. The request for a
variance should include supportive data which show that the toxicity of the effluent samples is not reduced
because of the increased holding temperature.
\17\ Samples collected for the determination of trace level mercury (100 ng/L) using EPA Method 1631 must be
collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48
hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
sample bottle. Samples collected for dissolved trace level mercury should be filtered in the laboratory.
However, if circumstances prevent overnight shipment, samples should be filtered in a designated clean area in
the field in accordance with procedures given in Method 1669. Samples that have been collected for
determination of total or dissolved trace level mercury must be analyzed within 90 days of sample collection.


[38 FR 28758, Oct. 16, 1973]

Editorial Note: For Federal Register citations affecting §136.3, see the List of CFR Sections Affected, which appears in the Finding Aids section of the printed volume and on GPO Access.

§ 136.4 Application for alternate test procedures.
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(a) Any person may apply to the Regional Administrator in the Region where the discharge occurs for approval of an alternative test procedure.

(b) When the discharge for which an alternative test procedure is proposed occurs within a State having a permit program approved pursuant to section 402 of the Act, the applicant shall submit his application to the Regional Administrator through the Director of the State agency having responsibility for issuance of NPDES permits within such State.

(c) Unless and until printed application forms are made available, an application for an alternate test procedure may be made by letter in triplicate. Any application for an alternate test procedure under this paragraph (c) shall:

(1) Provide the name and address of the responsible person or firm making the discharge (if not the applicant) and the applicable ID number of the existing or pending permit, issuing agency, and type of permit for which the alternate test procedure is requested, and the discharge serial number.

(2) Identify the pollutant or parameter for which approval of an alternate testing procedure is being requested.

(3) Provide justification for using testing procedures other than those specified in Table I.

(4) Provide a detailed description of the proposed alternate test procedure, together with references to published studies of the applicability of the alternate test procedure to the effluents in question.

(d) An application for approval of an alternate test procedure for nationwide use may be made by letter in triplicate to the Director, Analytical Methods Staff, Office of Science and Technology (4303), Office of Water, U.S. Environmental Protection Agency, 1200 Pennsylvania Ave., NW., Washington, DC 20460. Any application for an alternate test procedure under this paragraph (d) shall:

(1) Provide the name and address of the responsible person or firm making the application.

(2) Identify the pollutant(s) or parameter(s) for which nationwide approval of an alternate testing procedure is being requested.

(3) Provide a detailed description of the proposed alternate procedure, together with references to published or other studies confirming the general applicability of the alternate test procedure to the pollutant(s) or parameter(s) in waste water discharges from representative and specified industrial or other categories.

(4) Provide comparability data for the performance of the proposed alternate test procedure compared to the performance of the approved test procedures.

[38 FR 28760, Oct. 16, 1973, as amended at 41 FR 52785, Dec. 1, 1976; 62 FR 30763, June 5, 1997]

§ 136.5 Approval of alternate test procedures.
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(a) The Regional Administrator of the region in which the discharge will occur has final responsibility for approval of any alternate test procedure proposed by the responsible person or firm making the discharge.

(b) Within thirty days of receipt of an application, the Director will forward such application proposed by the responsible person or firm making the discharge, together with his recommendations, to the Regional Administrator. Where the Director recommends rejection of the application for scientific and technical reasons which he provides, the Regional Administrator shall deny the application, and shall forward a copy of the rejected application and his decision to the Director of the State Permit Program and to the Director of the Analytical Methods Staff, Washington, DC.

(c) Before approving any application for an alternate test procedure proposed by the responsible person or firm making the discharge, the Regional Administrator shall forward a copy of the application to the Director of the Analytical Methods Staff, Washington, DC.

(d) Within ninety days of receipt by the Regional Administrator of an application for an alternate test procedure, proposed by the responsible person or firm making the discharge, the Regional Administrator shall notify the applicant and the appropriate State agency of approval or rejection, or shall specify the additional information which is required to determine whether to approve the proposed test procedure. Prior to the expiration of such ninety day period, a recommendation providing the scientific and other technical basis for acceptance or rejection will be forwarded to the Regional Administrator by the Director of the Analytical Methods Staff, Washington, DC. A copy of all approval and rejection notifications will be forwarded to the Director, Analytical Methods Staff, Washington, DC, for the purposes of national coordination.

(e) Approval for nationwide use. (1) Within sixty days of the receipt by the Director of the Analytical Methods Staff, Washington, DC, of an application for an alternate test procedure for nationwide use, the Director of the Analytical Methods Staff shall notify the applicant in writing whether the application is complete. If the application is incomplete, the applicant shall be informed of the information necessary to make the application complete.

(2) Within ninety days of the receipt of a complete package, the Analytical Methods Staff shall perform any analysis necessary to determine whether the alternate method satisfies the applicable requirements of this part, and the Director of the Analytical Methods Staff shall recommend to the Administrator that he/she approve or reject the application and shall also notify the applicant of such recommendation.

(3) As expeditiously as practicable, an alternate method determined by the Administrator to satisfy the applicable requirements of this part shall be proposed by EPA for incorporation in subsection 136.3 of 40 CFR part 136. EPA shall make available for review all the factual bases for its proposal, including any performance data submitted by the applicant and any available EPA analysis of those data.

(4) Following a period of public comment, EPA shall, as expeditiously as practicable, publish in the Federal Register a final decision to approve or reject the alternate method.

[38 FR 28760, Oct. 16, 1973, as amended at 41 FR 52785, Dec. 1, 1976; 55 FR 33440, Aug. 15, 1990; 62 FR 30763, June 5, 1997]

Appendix A to Part 136—Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater
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Method 601—Purgeable Halocarbons

1. Scope and Application

1.1 This method covers the determination of 29 purgeable halocarbons.

The following parameters may be determined by this method:



------------------------------------------------------------------------
STORET
Parameter No. CAS No.
------------------------------------------------------------------------
Bromodichloromethane........................... 32101 75-27-4
Bromoform...................................... 32104 75-25-2
Bromomethane................................... 34413 74-83-9
Carbon tetrachloride........................... 32102 56-23-5
Chlorobenzene.................................. 34301 108-90-7
Chloroethane................................... 34311 75-00-3
2-Chloroethylvinyl ether....................... 34576 100-75-8
Chloroform..................................... 32106 67-66-3
Chloromethane.................................. 34418 74-87-3
Dibromochloromethane........................... 32105 124-48-1
1,2-Dichlorobenzene............................ 34536 95-50-1
1,3-Dichlorobenzene............................ 34566 541-73-1
1,4-Dichlorobenzene............................ 34571 106-46-7
Dichlorodifluoromethane........................ 34668 75-71-8
1,1-Dichloroethane............................. 34496 75-34-3
1,2-Dichloroethane............................. 34531 107-06-2
1,1-Dichloroethane............................. 34501 75-35-4
trans-1,2-Dichloroethene....................... 34546 156-60-5
1,2-Dichloropropane............................ 34541 78-87-5
cis-1,3-Dichloropropene........................ 34704 10061-01-5
trans-1,3-Dichloropropene...................... 34699 10061-02-6
Methylene chloride............................. 34423 75-09-2
1,1,2,2-Tetrachloroethane...................... 34516 79-34-5
Tetrachloroethene.............................. 34475 127-18-4
1,1,1-Trichloroethane.......................... 34506 71-55-6
1,1,2-Trichloroethane.......................... 34511 79-00-5
Tetrachloroethene.............................. 39180 79-01-6
Trichlorofluoromethane......................... 34488 75-69-4
Vinyl chloride................................. 39715 75-01-4
------------------------------------------------------------------------


1.2 This is a purge and trap gas chromatographic (GC) method applicable to the determination of the compounds listed above in municipal and industrial discharges as provided under 40 CFR 136.1. When this method is used to analyze unfamiliar samples for any or all of the compounds above, compound identifications should be supported by at least one additional qualitative technique. This method describes analytical conditions for a second gas chromatographic column that can be used to confirm measurements made with the primary column. Method 624 provides gas chromatograph/mass spectrometer (GC/MS) conditions appropriate for the qualitative and quantitative confirmation of results for most of the parameters listed above.

1.3 The method detection limit (MDL, defined in Section 12.1)1 for each parameter is listed in Table 1. The MDL for a specific wastewater may differ from those listed, depending upon the nature of interferences in the sample matrix.

1.4 Any modification of this method, beyond those expressly permitted, shall be considered as a major modification subject to application and approval of alternate test procedures under 40 CFR 136.4 and 136.5.

1.5 This method is restricted to use by or under the supervision of analysts experienced in the operation of a purge and trap system and a gas chromatograph and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this method using the procedure described in Section 8.2.

2. Summary of Method

2.1 An inert gas is bubbled through a 5-mL water sample contained in a specially-designed purging chamber at ambient temperature. The halocarbons are efficiently transferred from the aqueous phase to the vapor phase. The vapor is swept through a sorbent trap where the halocarbons are trapped. After purging is completed, the trap is heated and backflushed with the inert gas to desorb the halocarbons onto a gas chromatographic column. The gas chromatograph is temperature programmed to separate the halocarbons which are then detected with a halide-specific detector.2,3

2.2 The method provides an optional gas chromatographic column that may be helpful in resolving the compounds of interest from interferences that may occur.

3. Interferences

3.1 Impurities in the purge gas and organic compounds outgassing from the plumbing ahead of the trap account for the majority of contamination problems. The analytical system must be demonstrated to be free from contamination under the conditions of the analysis by running laboratory reagent blanks as described in Section 8.1.3. The use of non-Teflon plastic tubing, non-Teflon thread sealants, or flow controllers with rubber components in the purge and trap system should be avoided.

3.2 Samples can be contaminated by diffusion of volatile organics (particularly fluorocarbons and methylene chloride) through the septum seal ilto the sample during shipment and storage. A field reagent blank prepared from reagent water and carried through the sampling and handling protocol can serve as a check on such contamination.

3.3 Contamination by carry-over can occur whenever high level and low level samples are sequentially analyzed. To reduce carry-over, the purging device and sample syringe must be rinsed with reagent water between sample analyses. Whenever an unusually concentrated sample is encountered, it should be followed by an analysis of reagent water to check for cross contamination. For samples containing large amounts of water-soluble materials, suspended solids, high boiling compounds or high organohalide levels, it may be necessary to wash out the purging device with a detergent solution, rinse it with distilled water, and then dry it in a 105°C oven between analyses. The trap and other parts of the system are also subject to contamination; therefore, frequent bakeout and purging of the entire system may be required. (continued)