Section 327 IAC 8-2-4.2 - Analytical methods for inorganic chemical testingAuthority: IC 13-13-5; IC 13-14-8-7; IC 13-14-9; IC 13-18-3; IC 13-18-16
Affected: IC 13-11-2; IC 13-14-8; IC 13-18-1; IC 13-18-2
Sec. 4.2.
(a) Analyses conducted to determine compliance with section 4 of this rule shall be made in accordance with one (1) of the following methods* for each contaminant or with the alternative methods listed in Appendix A to Subpart C of 40 CFR 141. Criteria for analyzing arsenic, barium, beryllium, cadmium, calcium, chromium, copper, lead, nickel, selenium, sodium, and thallium with digestion or directly without digestion, and other analytical test procedures are contained in Technical Notes on Drinking Water Methods, EPA-600/R-94-173, October 1994. This document is available from the National Service Center for Environmental Publications (NSCEP), P.O. Box 42419, Cincinnati, OH 45242-0419 or http://www.epa.gov/nscep/: (1) Antimony as follows: (A) Atomic absorption1; furnace, Method 3113B*.(B) Atomic absorption; platform, Method 200.9*.(C) ICP-mass spectrometry, Method 200.8*.(D) Hydride-atomic absorption, Method D 3697-92*.(2) Arsenic* as follows: (A) Atomic absorption; furnace, Method D 2972-97C*, Method D 2972-03C*, Method 3113 B-99*, or Method 3113B*.(B) Hydride-atomic adsorption, Method D 2972-97B*, Method 1972-03C, Method 3114 B-97*, or Method 3114B*.(C) Atomic absorption, platform1, Method 200.92*.(D) ICP-mass spectrometry, Method 200.82*.(3) Asbestos, transmission electron microscopy, Method 100.1* or Method 100.2*.(4) Barium as follows: (A) Atomic absorption; furnace, Method 3113B*.(B) Atomic absorption; direct, Method 3111D*.(C) Inductively coupled plasma, Method 200.7* or Method 3120B*.(D) ICP-mass spectrometry, Method 200.8*.(5) Beryllium as follows:(A) Atomic absorption; furnace, Method D 3645-97B or Method 3113B.(B) Atomic absorption; platform, Method 200.9*.(C) Inductively coupled plasma, Method 200.7* or Method 3120B*.(D) ICP-mass spectrometry, Method 200.8.(6) Cadmium as follows:(A) Atomic absorption; furnace, Method 3113B*.(B) Inductively coupled plasma1, Method 200.7*.(C) ICP-mass spectrometry, Method 200.8*.(D) Atomic absorption; platform, Method 200.9*.(7) Chromium as follows: (A) Atomic absorption; furnace, Method 3113B*.(B) Inductively coupled plasma, Method 200.7* or Method 3120B*.(C) ICP-mass spectrometry, Method 200.8*.(D) Atomic absorption; platform, Method 200.9*.(8) Cyanide as follows: (A) Manual distillation followed by: (i) Spectrophotometric; amenable, Method D 2036-98B* or Method 4500-CN-G*.(ii) Spectrophotometric; manual, D 2036-98A*, Method 4500-CN-E*, or Method I-3300-85*.(iii) Spectrophotometric; semiautomated, Method 335.4*.(B) Selective electrode, Method 4500-CN-F*.(C) UV/Distillation/Spectrophotometric; Method Kelada 01.(D) Distillation/Spectrophotometric; Method QuikChem 10-204-00-1 -X.(9) Fluoride as follows: (A) Ion chromatography, Method 300.0*, Method D 4327-97*, or Method 4110B*.(B) Manual distillation; color. SPADNS, Method 4500F-B, D*.(C) Manual electrode, Method D 1179-93B* or Method 4500F-C*.(D) Automated electrode, Method 380-75WE*.(E) Automated alizarin, Method 4500F-E* or Method 129-71W*.(10) Mercury as follows: (A) Manual cold vapor, Method 245.1, Method D 3223-91*, or Method 3112B*.(B) Automated cold vapor, Method 245.2*.(C) ICP-mass spectrometry, Method 200.8*.(11) Nickel as follows:(A) Atomic absorption; furnace, Method 3113B*.(B) Atomic absorption; platform, Method 200.9.(C) Atomic absorption; direct, Method 3111B*.(D) Inductively coupled plasma, Method 200.7* or Method 3120B*.(E) ICP-mass spectrometry, Method 200.8*.(12) Nitrate as follows:(A) Manual cadmium reduction, Method D 3867-90B* or Method 4500-NO3-E*.(B) Automated cadmium reduction, Method 353.2*, Method D 3867-90A*, or Method 4500-NO3-F*.(C) Ion selective electrode, Method 4500-NO3-D* or Method 601*.(D) Ion chromatography, Method 300.0*, Method D 4327-97*, Method 4110B*, or Method B-1011*.(13) Nitrite as follows: (A) Ion chromatography, Method 300.0*, Method D 4327-97*, Method 4110B*, or Method B-1011*.(B) Automated cadmium reduction, Method 353.2*, Method D 3867-90A*, or Method 4500-NO3-F*.(C) Manual cadmium reduction, Method D 3867-90B* or Method 4500-NO3-E*.(D) Spectrophotometric, Method 4500-NO2-B*.(14) Selenium as follows: (A) Hydride-atomic absorption, Method D 3859-98A* or Method 3114B*.(B) ICP-mass spectrophotometry, Method 200.8*.(C) Atomic absorption; platform, Method 200.9*.(D) Atomic absorption; furnace, Method D 3859-98B* or Method 3113B*.(15) Thallium as follows: (A) Atomic absorption; platform1, Method 200.9*.(B) ICP-mass spectrometry, Method 200.8*. 1 Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2× preconcentration step during sample digestion, MDLs determined when samples are analyzed by direct analysis, that is, no sample digestion, will be higher. For direct analysis of cadmium by Method 200.7, sample preconcentration using pneumatic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony and thallium by Method 200.9 and antimony by Method 3113 B unless multiple in-furnace depositions are made.2 If ultrasonic nebulization is used in the determination of arsenic by Method 200.8, the arsenic must be in the pentavalent state to provide uniform signal response. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain one (1) mg/l of sodium hypochlorite.(b) Analysis under this section shall only be conducted by laboratories that have been certified by EPA or the commissioner. Laboratories may conduct sample analyses under provisional certification until January 1, 1996. To receive certification to conduct analyses for antimony, arsenic, asbestos, barium, beryllium, cadmium, chromium, cyanide, fluoride, mercury, nickel, nitrate, nitrite, selenium, and thallium, the laboratory must do the following: (1) Successfully analyze PE samples provided by EPA, the commissioner, or by a third party with approval of the EPA or the commissioner, at least once a year.(2) For each contaminant that has been included in the PE sample and for each method for which the laboratory desires certification achieve quantitative results on the analyses that are within the following acceptance limits: | |
| Contaminant | Acceptance Limit |
| Antimony | ±30% at >0.006 mg/l |
| Arsenic1 | ± 30% at > 0.003 mg/l |
| Asbestos | 2 standard deviations based on study statistics |
| Barium | ±15% at >0.15 mg/l |
| Beryllium | ±15% at >0.001 mg/l |
| Cadmium | ±20% at >0.002 mg/l |
| Chromium | ±15% at >0.01 mg/l |
| Cyanide | ±25% at >0.1 mg/l |
| Fluoride | ±10% at >1 to 10 mg/l |
| Mercury | ±30% at >0.0005 mg/l |
| Nickel | ±15% at >0.01 mg/l |
| Nitrate | ±10% at >0.4 mg/l |
| Nitrite | ±15% at >0.4 mg/l |
| Selenium | ±20% at >0.01 mg/l |
| Thallium | ±30% at >0.002 mg/l |
| 1Acceptance limit effective January 1, 2006. Until then, limit should be two (2) standard deviations based on study statistics. |
*Methods referenced in this section may be obtained as follows:
(1) Method 245.2, "Methods for Chemical Analysis or Water and Wastes", EPA-600/ 4-79-020, March 1983, available at NTIS, PB84-128677.(2) Methods 200.8, 200.9, 200.7, and 245.1 may be found in "Methods for the Determination of Metals in Environmental Samples-Supplement I", EPA-600/94-111, May 1994, available from NTIS, PB95-125472, 800-553-6847.(3) Methods D 3697-92, D 1179-93B, D 3223-91, D 3867-90A, D 3867-90B, D 3859-93A, and D 3859-93B, may be found in "Annual Book of ASTM Standards", 1994 and 1996, Vols. 11.01 and 11.02, American Society for Testing and Materials, available from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania 19428. Any year containing the cited version of the method may be used.(4) Methods D 2972-97C, D 2972-97B, D 3645-97B, D 2036-98A, D 2036-98B, D 4327-97, D 3859-98A, and D 3859-98B may be found in the "Annual Book of ASTM Standards, 1999, Vols. 11.01 and 11.02, American Society for Testing and Materials, available from the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania 19428. Any year containing the cited version of the method may be used.(5) Methods 3113B, 3114B, 3111D, and 3111B may be found in "18th Edition of Standard Methods for the Examination of Water and Wastewater", 1992, or "19th Edition of Standard Methods for the Examination of Water and Wastewater", 1995, American Public Health Association, available from the American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005. Either edition may be used.(6) Methods 3120B, 4500-CN-C, 4500-CN-G, 4500-CN-E, 4500-CN-F, 4110B, 4500F-B, 4500-F-D, 4500F-C, 4500F-E, 3112B, 4500-NO3-F, 4500-NO3-D, 4500-NO3-E, and 4500-NO2-B may be found in "18th Edition of Standard Methods for the Examination of Water and Wastewater", 1992, "19th Edition of Standard Methods for the Examination of Water and Wastewater", 1995, or "20th Edition of Standard Methods for the Examination of Water and Wastewater", 1998, American Public Health Association, available from the American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005. The cited methods published in any of the three (3) editions may be used.(7) Method I-3300-85 may be found in Techniques of Water Resources Investigation of the U.S. Geological Survey, Book 5, Chapter A-1, 3rd Edition, 1989, available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, Colorado 80225-0425.(8) Methods 335.4, 300.0, and 353.2 may be found in "Methods for the Determination of Inorganic Substances in Environmental Samples", EPA-600/R-93-100, August 1993, available from NTIS, PB94-120821.(9) Method 601 may be found in Technical Bulletin 601 "Standard Method of Test for Nitrate in Drinking Water", July 1994, PN 221890-001, Analytical Technology, Inc., available from ATI Orion, 529 Main Street, Boston, Massachusetts 02129.(10) Method B-1011 may be found in "Waters Test Method for Determination of Nitrate/Nitrite in Water Using Single Column Ion Chromatography", August 1987, available from Waters Corporation, 34 Maple Street, Milford, Massachusetts 01757.(11) Method 100.1 may be found in "Analytical Methods for Determination of Asbestos Fibers in Water", EPA-600/ 4-83-043, EPA, September 1983, available from NTIS, PB83-260471.(12) Method 100.2 may be found in "Determination of Asbestos Structure Over 10-µm in Length in Drinking Water", EPA-600/R-94-134, June 1994, available from NTIS, PB94-201902.(13) Method 129-71W may be found in "Fluoride in Water and Wastewater", December 1972, Technicon Industrial Systems, available from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, Illinois 60089.(14) Method 380-75WE may be found in "Fluoride in Water and Wastewater", February 1976, Technicon Industrial Systems, available from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, Illinois 60089.(15) Method Kelada 01 may be found in "Kelada Automated Test Methods for Total Cyanide, Acid Dissolvable Cyanide, and Thiocyanate", Rev 1.2, August 2001, EPA 821-B-01-099, available from the National Technical Information Service (NTIS), PB 2001-108275, 5285 Port Royal Road, Springfield, Virginia 22161, 800-553-6847.(16) Method QuikChem 10-204-00-1 -X may be found in "Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST and determination of cyanide by flow injection analysis", Rev 2.1, November 30, 2000, available from Lachat Industries, 6645 West Mill Road, Milwaukee, Wisconsin 53218, 414-358-4200. These methods are also available for copying at the Indiana Department of Environmental Management, Office of Water Quality, 100 North Senate Avenue, Room N1255, Indianapolis, Indiana 46204.
Water Pollution Control Division; 327 IAC 8-2-4.2; filed Dec 28, 1990, 5:10 p.m.: 14 IR 1008; errata filed Aug 6, 1991, 3:45 p.m.: 14 IR 2258; filed Aug 24, 1994, 8:15 a.m.: 18 IR 29; errata filed Oct 11, 1994, 2:45 p.m.: 18 IR 531; filed Aug 25, 1997, 8:00 a.m.: 21 IR 40; filed Jul 23, 2001, 1:02 p.m.: 24 IR 3951; filed Jun 13, 2005, 2:30 p.m.: 28 IR 3196; errata filed Jul 6, 2005, 3:15 p.m.: 28 IR 3582; errata filed Aug 22, 2005, 2:55 p.m.: 29 IR 30; filed Feb 25, 2013, 8:36 a.m.: 20130327-IR-327110667FRA