Section 327IAC8-2-45. Analytical methods; lead and copper

   (a) Analysis for lead, copper, pH, conductivity, calcium, alkalinity, orthophosphate, silica, and temperature shall be conducted using the following methods or with the alternative methods listed in Appendix A to Subpart C of 40 CFR 141:

(1) Lead as follows:

(A) Atomic absorption; furnace technique, Method D 3559-90D¹*, Method D 3559-96*, or Method 3113B¹*.

(B) Inductively-coupled plasma; mass spectrometry, Method 200.8*.

(C) Atomic absorption; platform furnace technique, Method 200.9¹*.

(D) Differential pulse anodic stripping voltammetry, Method 1001*.

(2) Copper as follows:

(A) Atomic absorption; furnace technique, Method D 1688-90C*, Method D 1688-95C*, or Method 3113B*.

(B) Atomic absorption; direct aspiration, Method D 1688-90A*, Method D 1688-95A*, or Method 3111B*.

(C) Inductively-coupled plasma; Method 200.7* or Method 3120B*.

(D) Inductively-coupled plasma; mass spectrometry, Method 200.8*.

(E) Atomic absorption; platform furnace, Method 200.9*.

(3) pH, electrometric, Method 150.1*, Method 150.2*, Method D 1293-84*, Method D 1293-95*, or Method 4500-H⁺-B*.

(4) Conductivity, conductance, Method D 1125-91A*, Method D 1125-95A*, or Method 2510B*.

(5) Calcium as follows:

(A) EDTA titrimetric, Method D 511-93A* or Method 3500-Ca-D*.

(B) Atomic absorption; direct aspiration, Method D 511-93B* or Method 3111-B*.

(C) Inductively-coupled plasma, Method 200.7 or Method 3120B*.

(6) Alkalinity as follows:

(A) Titrimetric, Method D 1067-92B* or Method 2320B.

(B) Electrometric titration, Method I-1030-85*.

(7) Orthophosphate, unfiltered, no digestion or hydrolysis as follows:

(A) Colorimetric, automated, ascorbic acid, Method 365.1* or Method 4500-P-F*.

(B) Colorimetric, ascorbic acid, single reagent, Method D 515-88A* or Method 4500-P-E*.

(C) Colorimetric, phosphomolybdate, Method I-1601-85* or automated-segmented flow, Method I-2601-90*, or automated discrete, Method I-2598-85*.

(D) Ion chromatography, Method 300.0*, Method D 4327-97*, or Method 4110B*.

(8) Silica as follows:

(A) Colorimetric, molybdate blue, Method I-1700-85 or automated-segmented flow, Method I-2700-85*.

(B) Colorimetric, Method D 859-88* or Method D 859-95*.

(C) Molybdosilicate, Method 4500-Si-D* or Method 4500-SiO₂ C*.

(D) Heteropoly blue, Method 4500-Si-E* or Method 4500-SiO₂ D*.

(E) Automated method for molybdate-reactive silica, Method 4500-Si-F* or Method 4500-SiO₂ E*.

(F) Inductively-coupled plasma, Method 200.7* or Method 3120B*.

(9) Temperature, thermometric, Method 2550*.

¹Because 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. Preconcentration may be required to direct analysis of lead by Method 200.9, Method 3113 B, and Method D 3559-90D unless multiple in-furnace depositions are made.

  (b) Analyses for alkalinity, calcium, conductivity, orthophosphate, pH, silica, and temperature may be performed by any person acceptable to the commissioner. Analyses under this section for lead and copper shall only be conducted by laboratories that have been certified by the EPA or the commissioner. To obtain certification to conduct analysis for lead and copper, laboratories must do the following:

(1) Successfully analyze (PE) samples that include lead and copper provided by or acceptable to EPA or the commissioner at least once each year by each method for which the laboratory desires certification.

(2) Achieve quantitative acceptance limits as follows:

(A) For lead, plus or minus thirty percent (30%) of the actual amount in the PE sample when the actual amount is greater than or equal to five-hundredths (0.05) milligram per liter.

(B) For copper, plus or minus ten percent (10%) of the actual amount in the PE sample when the actual amount is greater than or equal to five-thousandths (0.005) milligram per liter.

(3) Achieve the method detection limit for lead of one-thousandth (0.001) milligram per liter according to the procedures in Appendix B of 40 CFR 136 (July 1, 1991). This need only be done if the laboratory will be processing source water composite samples under section 39 of this rule.

(4) Be currently certified by EPA or the state to perform analyses to the specifications described in this subsection.

  (c) The commissioner has the authority to allow the use of previously collected monitoring data for purposes of monitoring if the data were collected and analyzed in accordance with sections 36 through 44 of this rule, this section, and sections 46 and 47 of this rule.

  (d) All lead levels measured between the practical quantitation level and the method detection limit must be either reported as measured or they can be reported as one-half (1/2) the practical quantitation level (twenty-five ten-thousandths (0.0025) milligram per liter). All levels below the lead method detection level must be reported as zero (0).

  (e) All copper levels measured between the practical quantitation level and the method detection limit must be either reported as measured or they can be reported as one-half (1/2) the practical quantitation level (twenty-five thousandths (0.025) milligram per liter). All levels below the copper method detection limit must be reported as zero (0).

¹For analyzing lead and copper, the technique applicable to total metals must be used and samples cannot be filtered.

  *Methods referenced in this section may be obtained as follows:

(1) Methods 150.1 and 150.2, may be found in "Methods for Chemical Analysis of Water and Wastes", EPA/600/4-79/020, March 1983, available from NTIS, PB84-128677, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161.

(2) Methods 200.7, 200.8, and 200.9 may be found in "Methods for the Determination of Metals in Environmental Samples-Supplement 1", EPA-600/R-94-111, May 1994, available from NTIS, PB95-125472, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161.

(3) Methods D3559-90D, D1688-90C, D1688-90A, D1293-84, D1125-91A, and D859-88 may be found in "Annual Book of ASTM Standards", Vols. 11.01, 1994, 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 D1067-92B, D511-93A, D511-93B, D1688-95C, D1688-95A, D1125-95A, D3559-96, D515-88A, D4327-91, D1293-95, and D859-95 may be found in "Annual Book of ASTM Standards, Vols. 11.01 and 11.02, 1994 and 1996, 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, 4500-Si-D, 4500-Si-E, and 4500-Si-F may be found in "Standard Methods for the Examination of Water and Wastewater", 18th Edition, 1992, and "Standard Methods for the Examination of Water and Wastewater", 19th Edition, 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 2320B, 3111B, 3120B, 4500-H⁺-B, 2510B, 3500-Ca-D, 2320B, 4500-P-F, 4500-P-E, 4110B, and 2550 may be found in "Standard Methods for the Examination of Water and Wastewater", 18th Edition, 1992, and "Standard Methods for the Examination of Water and Wastewater", 19th Edition, 1995, and "Standard Methods for the Examination of Water and Wastewater", 20th Edition, 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) Methods 4500-SiO₂ C, 4500-SiO₂ D, and 4500-SiO₂ E may be found in "Standard Methods for the Examination of Water and Wastewater", 20th Edition, 1998, American Public Health Association, 1015 Fifteenth Street NW, Washington, D.C. 20005.

(8) Methods I-1030-85, I-1601-85, I-2598-85, I-1700-85, and I-2700-85 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.

(9) Method I-2601-90 may be found in "Methods for 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 93-125, 1993, available from Information Services, U.S. Geological Survey, Federal Center, Box 25286, Denver, Colorado 80225-0425.

(10) Methods 365.1 and 300.0 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, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161.

(11) Method 1001 is available from Palintest, LTC, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, Kentucky 41018 or from the Hach Company, P.O. Box 389, Loveland, Colorado 80539-0389.

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 8-2-45; filed Aug 24, 1994, 8:15 a.m.: 18 IR 82; errata filed Oct 11, 1994, 2:45 p.m: 18 IR 532; filed Aug 25, 1997, 8:00 a.m.: 21 IR 72; errata filed Dec 10, 1997, 3:45 p.m.: 21 IR 1349; filed Jul 23, 2001, 1:02 p.m.: 24 IR 3978; errata filed Jul 25, 2001, 3:25 p.m.: 24 IR 3991; filed Jun 13, 2005, 2:30 p.m.: 28 IR 3218; errata filed Jul 6, 2005, 3:15 p.m.: 28 IR 3583; filed May 7, 2010, 9:30 a.m.: 20100602-IR-327080198FRA; filed Feb 25, 2013, 8:36 a.m.: 20130327-IR-327110667FRA)