Section 809.113. Sample collection and analytical requirements for inorganic contaminants.

 

(1)   analytical methods. Analyses conducted to determine compliance with s. NR 809.11 shall be made in accordance with methods listed in Table A. - See PDF for table

Copies of the documents may be obtained from the sources listed below. Information regarding obtaining these documents can be obtained from the Safe Drinking Water Hotline at 800–426–4791, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html .

1   "Methods for Chemical Analysis of Water and Wastes," EPA/600/4–79/020, March 1983. Available at NTIS, PB84–128677.

2   "Methods for the Determination of Metals in Environmental Samples—Supplement I," EPA/600/R–94/111, May 1994. Available at NTIS, PB95–125472.

3   Annual Book of ASTM Standards, 1994, 1996, 1999, or 2003, Vols. 11.01 and 11.02, ASTM International; any year containing the cited version of the method may be used. The previous versions of D1688–95A, D1688–95C (copper), D3559–95D (lead), D1293–95 (pH), D1125–91A (conductivity) and D859–94 (silica) are also approved. These previous versions D1688–90A, C; D3559–90D, D1293–84, D1125–91A and D859–88, respectively are located in the Annual Book of ASTM Standards, 1994, Vol. 11.01. Copies may be obtained from ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

4   Standard Methods for the Examination of Water and Wastewater, 18th edition (1992), 19th edition (1995), 20th edition (1998), 21 st edition (2005), or 22 nd edition (2012). American Public Health Association, 1015 Fifteenth Street, NW., Washington, DC 20005. The cited methods published in any of these three editions may be used, except that the versions of 3111 B, 3111 D, 3113 B and 3114 B in the 20th edition may not be used.

5 Method I–2601–90, Methods for Analysis by the U.S. Geological Survey National Water Quality Laboratory—Determination of Inorganic and Organic Constituents in Water and Fluvial Sediment, Open File Report 93–125, 1993; For Methods I–1030–85; I–1601–85; I–1700– 85; I–2598–85; I–2700–85; and I–3300–85 See 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, CO 80225–0425.

6 "Methods for the Determination of Inorganic Substances in Environmental Samples," EPA/600/R–93/100, August 1993. Available at NTIS, PB94–120821.

7 The procedure shall be done in accordance with the Technical Bulletin 601 " Standard Method of Test for Nitrate in Drinking Water," July 1994, PN 221890–001, Analytical Technology, Inc. Copies may be obtained from ATI Orion, 529 Main Street, Boston, MA 02129.

8 Method B–1011, "Waters Test Method for Determination of Nitrite/Nitrate in Water Using Single Column Ion Chromatography," August 1987. Copies may be obtained from Waters Corporation, Technical Services Division, 34 Maple Street, Milford, MA 01757, Telephone: [phone], Fax: [phone].

9 Method 100.1, "Analytical Method For Determination of Asbestos Fibers in Water," EPA/600/4–83/043, EPA, September 1983. Available at NTIS, PB83–260471.

10 Method 100.2, "Determination of Asbestos Structure Over 10-ìm In Length In Drinking Water," EPA/600/R–94/134, June 1994. Available at NTIS, PB94–201902.

11 Industrial Method No. 129–71W, "Fluoride in Water and Wastewater," December 1972, and Method No. 380–75WE, "Fluoride in Water and Wastewater," February 1976, Technicon Industrial Systems. Copies may be obtained from Bran & Luebbe, 1025 Busch Parkway, Buffalo Grove, IL 60089.

12 Unfiltered, no digestion or hydrolysis.

13 Because MDLs reported in EPA Methods 200.7 and 200.9 were determined using a 2x preconcentration step during sample digestion, MDLs determined when samples are analyzed by direct analysis ( i.e. , no sample digestion) will be higher. For direct analysis of cadmium and arsenic by Method 200.7, and arsenic by Method 3120 B, sample preconcentration using pneumatic nebulization may be required to achieve lower detection limits. Preconcentration may also be required for direct analysis of antimony, lead, and thallium by Method 200.9; antimony and lead by Method 3113 B; and lead by Method D3559–90D, unless multiple in-furnace depositions are made.

14 If ultrasonic nebulization is used in the determination of arsenic by Methods 200.7, 200.8, or SM 3120 B, the arsenic must be in the pentavalent state to provide uniform signal response. For Methods 200.7 and 3120 B, both samples and standards must be diluted in the same mixed acid matrix concentration of nitric and hydrochloric acid with the addition of 100 ìL of 30% hydrogen peroxide per 100 mL of solution. For direct analysis of arsenic with Method 200.8 using ultrasonic nebulization, samples and standards must contain 1 mg/L of sodium hypochlorite.

15 The description for Method Number 1001 for lead is available from Palintest, LTD, 21 Kenton Lands Road, P.O. Box 18395, Erlanger, KY 41018. Or from the Hach Company, P.O. Box 389, Loveland, CO 80539.

16 The description for the Kelada-01 Method, "Kelada Automated Test Methods for Total Cyanide, Acid Dissociable Cyanide, And Thiocyanate," Revision 1.2, August 2001, EPA # 821–B–01–009 for cyanide is available from the National Technical Information Service (NTIS), PB 2001–108275, 5285 Port Royal Road, Springfield, VA 22161. The toll free telephone number is 800–553–6847.

(2)   Sample collection. Sample collection for the inorganic contaminants under s. NR 809.11 (2) shall be conducted using the sample preservation, containers and maximum holding time procedures specified in Table B. In all cases, samples should be analyzed as soon after collection as possible. - See PDF for table

(3)   Laboratory certification. Analyses under this section shall only be conducted by laboratories that have received certification under ch. NR 149 or approval by EPA.

(a) To receive certification to conduct analyses for antimony, arsenic, asbestos, barium, beryllium, cadmium, cyanide, fluoride, mercury, nickel, nitrate, nitrite, selenium and thallium, a laboratory shall carry out annual analyses of performance evaluation samples approved by the department or EPA.

(b) For each contaminant that has been included in the performance evaluation sample and for each method for which a laboratory desires certification, the laboratory shall achieve quantitative results that are within the following acceptance limits: - See PDF for table

(4)   Composite sampling . Composite sampling for inorganic contaminants shall meet the following requirements:

(a) The department may reduce the total number of samples a public water system is required to analyze by allowing the use of compositing. Compositing shall only be permitted for entry points within a single public water system. Composite samples from a maximum of 5 entry points are allowed, provided that the detection limit of the method used for analysis is less than one-fifth of the MCL.

(b) Compositing of samples shall be done in the laboratory.

(c) If the concentration in the composite sample is greater than or equal to one-fifth of the MCL of any inorganic contaminant, a follow-up sample shall be taken from each entry point included in the composite and analyzed within 14 days. These samples shall be analyzed for the contaminants which exceeded one-fifth of the MCL in the composite sample.

(d) If duplicates of the original sample taken from each entry point used in the composite are available and the holding time listed in sub. (2) Table B has not been exceeded, the water supplier may use these instead of resampling. The duplicates shall be analyzed and the results reported to the department within 14 days of the composite analysis.

(e) The detection limits in Table C, are the detection limits that laboratories shall use for each analytical method and MCLs for inorganic contaminants specified in this section and s. NR 809.11 :

CR 09-073 : cr. Register November 2010 No. 659 , eff. 12-1-10; CR 15-049 : am. (1) Table A, (4) Table C Register March 2016 No. 723 , eff. 4-1-16.

Note

A 450–W UV lamp may be used in this method instead of the 550–W lamp specified if it provides performance within the quality control (QC) acceptance criteria of the method in a given instrument. Similarly, modified flow cell configurations and flow conditions may be used in the method, provided that the QC acceptance criteria are met. Microsoft Windows NT 6.1.7601 Service Pack 1 17   The description for the QuikChem Method 10–204– 00–1–X, "Digestion and distillation of total cyanide in drinking and wastewaters using MICRO DIST and determination of cyanide by flow injection analysis," Revision 2.1, November 30, 2000, for cyanide is available from Lachat Instruments, 6645 W. Mill Rd., Milwaukee, WI 53218. Telephone: [phone]. Microsoft Windows NT 6.1.7601 Service Pack 1 18   "Methods for the Determination of Organic and Inorganic Compounds in Drinking Water," Vol. 1, EPA 815–R–00– 014, August 2000. Available at NTIS, PB2000–106981. Microsoft Windows NT 6.1.7601 Service Pack 1 19   Method OIA–1677, DW "Available Cyanide by Flow Injection, Ligand Exchange, and Amperometry," January 2004. EPA–821–R–04–001, Available from ALPKEM, A Division of OI Analytical, P.O. Box 9010, College Station, TX 77842–9010. Microsoft Windows NT 6.1.7601 Service Pack 1 20   Sulfide levels below those detected using lead acetate paper may produce positive method interferences. Test samples using a more sensitive sulfide method to determine if a sulfide interference is present, and treat samples accordingly. Microsoft Windows NT 6.1.7601 Service Pack 1 21   Standard Methods Online are available at http://www.standardmethods.org . The year in which each method was approved by the Standard Methods Committee is designated by the last two digits in the method number. The methods listed are the only online versions that may be used. Microsoft Windows NT 6.1.7601 Service Pack 1 22   Method D6508, Rev. 2, "Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte," available from Waters Corp, 34 Maple St, Milford, MA, 01757, Telephone: [phone], Fax: [phone]. Microsoft Windows NT 6.1.7601 Service Pack 1 23   "Methods for the Determination of Inorganic Substances in Environmental Samples", EPA-600/R-93-100, August 1993, Available at NTIS, PB94-121811 Microsoft Windows NT 6.1.7601 Service Pack 1 24   GLI Method 2, "Turbidity", November 2, 1992, Great Lakes Instruments, Inc., 8855 North 55th Street, Milwaukee, Wisconsin 53223. Microsoft Windows NT 6.1.7601 Service Pack 1 25   EPA Method 200.5 Revision 4.2. "Determination of Trace Elements in Drinking Water by Axially Viewed Inductively Coupled Plasma-Atomic Emission Spectrometry." 2003. EPA/600/R-06/115. Available at http:/ www.epa.gov/nerlcwww/ordmeth.htm . Microsoft Windows NT 6.1.7601 Service Pack 1 26 Method ME355.01, Revision 1.0. "Determination of Cyanide in Drinking Water by GC/MS Headspace." May 26, 2009. Available at http://www.nemi.gov or from James Eaton , H & E Testing Laboratory, 221 State Street, Augusta, ME 04333. [phone] Microsoft Windows NT 6.1.7601 Service Pack 1 27 Hach Company Method, "Hach Company SPADNS 2 (Arsenite –free) Fluoride Method 10255-Spectrophotometric Measurement of Fluoride in Water and Wastewater," January 2011. 5600 Lindbergh Drive, P.O. Box 389, Loveland , Colorado 80539. Available at http://www.hach.com . Microsoft Windows NT 6.1.7601 Service Pack 1 28 Systea Easy (1-Reagent). "Systea Easy (1-Reagent) Nitrate Method," February 4, 2009. Available at http://www.nemi.gov or from Systea Scientific, LLC., 900 Jorie Blvd., Suite 35, Oak Brook, IL 60523. Microsoft Windows NT 6.1.7601 Service Pack 1 29 Mitchell Method M5271, Revision 1.1." Determination of Turbidity by Laser Nephelometry," March 5, 2009. Available at http://www.nemi.gov or from Leck Mitchell, PhD, PE, 656 Independence Valley Dr., Grand Junction, CO 81507. Microsoft Windows NT 6.1.7601 Service Pack 1 30 Mitchell Method M5331, Revision 1.1. "Determination of Turbidity by LED Nephelometry," March 5, 2009. Available at http://www.nemi.gov or from Leck Mitchell, PhD, PE, 656 Independence Valley Dr., Grand Junction, CO 81507. Microsoft Windows NT 6.1.7601 Service Pack 1 31 AMI Turbiwell. "Continuous Measurement of turbidity Using a SWAN AMI Turbiwell Turbidimeter," August 2009. Available at http://www.nemi.gov or from Markus Bernasconi, SWAN Analytische Instrumente AG, Studbachstrasse 13, CH-8340 Hinwil, Switzerland. Microsoft Windows NT 6.1.7601 Service Pack 1 32 Orion Method AQ4500, Revision 1.0. "Determination of Turbidity by LED Nephelometry," May 8, 2009. Available at http://www.nemi.gov or from Thermo Scientific, 166 Cummings Center, Beverly, MA 0`9`5, http://www.thermo.com . Microsoft Windows NT 6.1.7601 Service Pack 1 33 Hach FilterTrak Method 10133, "Determination of Turbidity by Laser Nephelomemtry," January 2000, Revision 2.0. Available from Hach Co., P.O. Box389, Loveland, CO 80539-0389. Microsoft Windows NT 6.1.7601 Service Pack 1 TABLE C
Detection Limits for Inorganic Contaminants - See PDF for table Microsoft Windows NT 6.1.7601 Service Pack 1 1 MFL = million fibers per liter >10 m m. Microsoft Windows NT 6.1.7601 Service Pack 1 2 Using a 2X preconcentration step as noted in Method 200.7. Lower MDLs may be achieved when using a 4X preconcentration. Microsoft Windows NT 6.1.7601 Service Pack 1 3 Screening method for total cyanides. Microsoft Windows NT 6.1.7601 Service Pack 1 4 Measures "free" cyanides when distillation, digestion, or ligand exchange is omitted. Microsoft Windows NT 6.1.7601 Service Pack 1 5 Lower MDLs are reported using stabilized temperature graphite furnace atomic absorption. Microsoft Windows NT 6.1.7601 Service Pack 1 6 The MDL reported for EPA method 200.9 (Atomic Absorption; Platform—Stabilized Temperature) was determined using a 2x concentration step during sample digestion. The MDL determined for samples analyzed using direct analyses ( i.e. , no sample digestion) will be higher. Using multiple depositions, EPA 200.9 is capable of obtaining MDL of 0.0001 mg/L. Microsoft Windows NT 6.1.7601 Service Pack 1 7 Using selective ion monitoring, EPA Method 200.8 (ICP-MS) is capable of obtaining a MDL of 0.0001 mg/L. Microsoft Windows NT 6.1.7601 Service Pack 1 8 Measures total cyanides when UV-digestor is used, and "free" cyanides when UV-digestor is bypassed. Microsoft Windows NT 6.1.7601 Service Pack 1