Chapter NR 219

Register April 2010 No. 652

Chapter NR 219

ANALYTICAL TEST METHODS AND PROCEDURES

NR 219.01   Purpose.

NR 219.02   Applicability.

NR 219.03   Definitions.

NR 219.033   Alternate test procedures.

NR 219.037   Laboratory certification or registration.

NR 219.04   Identification of test procedures.

Ch. NR 219 Note Note: A number of the references cited in this chapter are no longer in print. Copies of references which are out-of-print are available at any public library by inter-library loan.

NR 219.01 NR 219.01 Purpose. The purpose of this chapter is to establish analytical test methods, preservation procedures, requirements for laboratories, and procedures applicable to effluent limitations for discharges from point sources as authorized by ss. 299.11 and 283.55 (1), Stats.

NR 219.01 History History: Cr. Register, August, 1976, No. 248, eff. 9-1-76; am. Register, April, 1986, No. 364, eff. 8-28-86; am. Register, June, 1986, No. 366, eff. 7-1-86; am. Register, April, 1988, No. 388, eff. 5-1-88; corrections made under s. 13.93 (2m) (b) 7., Stats., Register, November, 1996, No. 491.

NR 219.02 NR 219.02 Applicability.

NR 219.02(1) (1) The procedures prescribed herein shall, except as provided in s. NR 219.037, be used in the determination of concentrations and quantities of pollutant parameters as required for:

NR 219.02(1)(a) (a) An application submitted to the department for a permit under ch. 283, Stats.

NR 219.02(1)(b) (b) Reports required to be submitted by dischargers in accordance with the conditions of issued permits.

NR 219.02(2) (2) Section NR 219.037 requires that laboratories conducting tests under this chapter be certified, registered, or approved under ch. NR 149.

NR 219.02 History History: Cr. Register, August, 1976, No. 248, eff. 9-1-76; am. Register, April, 1986, No. 364, eff. 8-28-86; am. (1) (intro.), Register, June, 1986, No. 366, eff. 7-1-86; correction in (1) (a) made under s. 13.93 (2m) (b) 7., Stats., Register, November, 1996, No. 491; correction in (2) made under s. 13.93 (2m) (b) 7., Stats., Register October 2002 No. 562; correction in (2) made under s. 13.93 (2m) (b) 7., Stats., Register November 2004 No. 587; CR 13-112: am. (1), (2) Register May 2015 No. 713, eff. 6-1-15.

NR 219.03 NR 219.03 Definitions. As used in this chapter:

NR 219.03(1) (1) “EPA” means the U.S. environmental protection agency.

NR 219.03(2) (2) “Department” means the department of natural resources.

NR 219.03(3) (3) “Sludge” is defined in ss. NR 204.03 (55) and 214.03 (34).

NR 219.03 History History: Cr. Register, August, 1976, No. 248, eff. 9-1-76; am. (1), (2), (3) and (4m), Register, January, 1978, No. 265, eff. 2-1-78; r. and recr. Register, June, 1986, No. 366, eff. 7-1-86; r. and recr. (1), r. (3) and (4), Register, November, 1992, No. 443, eff. 12-1-92: CR 04-033: cr. (3) Register November 2004 No. 587, eff. 12-1-04.

NR 219.033 NR 219.033 Alternate test procedures. Approvals of alternate test procedures for nationwide use and specific discharges are granted by EPA. The department may approve the use of an alternate test procedure on a case-by-case basis if the criteria for approval of the alternate procedure established in s. NR 149.42 are met. If the department or the EPA approves an alternate test procedure, it shall be considered equivalent to the approved method.

NR 219.033 Note Note: The federal requirements for alternate test procedure approval are given in 40 CFR 136.5.

NR 219.033 History History: Cr. Register, August, 1976, No. 248, eff. 9-1-76; r. and recr. January, 1978, No. 265, eff. 2-1-78; renum. from NR 219.04 and am. Register, June, 1986, No. 366, eff. 7-1-86; r. and recr. Register, November, 1992, No. 443, eff. 12-1-92; am. Register, February, 1996, No. 482, eff. 3-1-96; correction made under s. 13.92 (4) (b) 7., Stats., Register May 2009 No. 641, eff. 6-1-09; CR 13-112: renum. from 219.05 Register May 2015 No. 713, eff. 6-1-15.

NR 219.037 NR 219.037 Laboratory certification or registration. Bacteriological analyses of groundwater samples, and all radiological analyses shall be performed by the state laboratory of hygiene or at a laboratory certified or approved by the department of agriculture, trade and consumer protection. Other laboratory test results, including effluent toxicity, submitted to the department under a WPDES permit shall be performed by a laboratory certified or registered under ch. NR 149. The following tests are excluded from this requirement:

NR 219.037(1) (1) Temperature,

NR 219.037(2) (2) Turbidity,

NR 219.037(3) (3) Bacteria tests in wastewater effluent and sludges,

NR 219.037(4) (4) pH,

NR 219.037(5) (5) Chlorine residual,

NR 219.037(6) (6) Specific conductance,

NR 219.037(7) (7) Physical properties of soils and sludges,

NR 219.037(8) (8) Nutrient tests of soils and sludges,

NR 219.037(9) (9) Flow measurements.

NR 219.037 History History: Cr. Register, April, 1986, No. 364, eff. 8-28-86; renum. from NR 219.07 and am. (intro.) Register, November, 1992, No. 443, eff. 7-1-93; am. Register February, 1996, No. 482, eff. 3-1-96; correction in (intro.) made under s. 13.93 (2m) (b) 6., Stats., Register November 2004 No. 587; CR 13-112: renum. from 219.06 Register May 2015 No. 713, eff. 6-1-15.

NR 219.04 NR 219.04 Identification of test procedures.

NR 219.04(1) (1) Analytical test procedures. Parameters or pollutants, for which wastewater analytical methods are approved, are listed together with test procedure descriptions and references in tables A to H. Parameters or pollutants, for which sludge analytical methods are approved, are listed together with test procedure descriptions and references in table EM. The discharge values for the listed parameters shall be determined by one of the standard analytical test procedures identified in a table under this subsection or by an alternate test procedure established under ss. NR 219.033 and 149.42.

NR 219.04 Note Note: The laboratory performing the analyses on any samples will be certified for the applicable PFAS compounds in aqueous, sludge (biosolids), and tissue matrices in accordance with s. NR 149.41 by the Wisconsin Laboratory Certification Program established under s. 299.11, Stats. If the EPA Office of Water publishes a final approved 1600 series isotope dilution method for the analysis of PFAS in aqueous, sludge (biosolids), and tissue matrices, the department recommends use of the final approved EPA method.

NR 219.04(2) (2) Sample preservation procedures. Sample preservation techniques, container materials, and maximum allowable holding times for parameters identified in tables A to H are prescribed in table F. Sludge samples shall be preserved at the time of collection by cooling to less than or equal to 6°C where required. All samples requiring thermal preservation at less than or equal to 6°C shall be cooled immediately after collection, and the required temperature maintained during shipping. Any person may apply for a variance from the prescribed preservation procedures applicable to samples taken from a specific discharge. Applications for variances may be made by letters to the regional administrator and shall provide sufficient data to assure that the variance does not adversely affect the integrity of the sample. The regional administrator will make a decision on whether to approve or deny a variance within 90 days of receipt of the application.

NR 219.04(3) (3) Temperature reporting procedures. Samples cooled with ice packs or not in direct contact with ice during shipping shall be cooled to less than or equal to 6° C prior to shipping, and a temperature blank shall be submitted with the samples. Samples cooled during shipping with ice packs may not be recorded as received on ice. Samples may be recorded as received on ice only if solid ice is present in the cooler at the time the samples are received. If the samples are not received on ice, the laboratory shall record one of the following at the time of receipt:

NR 219.04(3)(a) (a) The temperature of an actual sample.

NR 219.04(3)(b) (b) The temperature of a temperature blank shipped with the samples.

NR 219.04(3)(c) (c) The temperature of the melt water in the shipping container.

NR 219.04(4) (4) Incorporation by reference. The materials in this section are incorporated by reference for the purposes of the permit program under ch. 283, Stats.

NR 219.04 Note Note: Copies of the publications referenced in Tables A-H are available for inspection at the offices of the department of natural resources and the legislative reference bureau. Many of these materials are also available through inter-library loan.

NR 219.04 History History: Cr. Register, June, 1986, No. 366, eff. 7-1-86; r. and recr. Tables B and E, Register, April, 1988, No. 388, eff. 5-1-88; am.; r. and recr. Tables A to F, Register, November, 1992, No. 443, eff. 12-1-92; am. (1), am. Tables A to F, Register, April, 1994, No. 460, eff. 5-1-94; am. (1) and (2), Tables A to F, cr. (3), Register, February, 1996, No. 482, eff. 3-1-96; CR 02-019: am. Table B Register October 2002 No. 562, eff. 11-1-02; CR 04-033: r. and recr. Table A, Table B, Table BM, Table C, Table D, Table E, Table EM, and Table F, cr. Table ES Register November 2004 No. 587, eff. 12-1-04; CR 04-101: am. Table A Note 29 Register May 2005 No. 593, eff. 6-1-05; CR 08-076: am. (2) and (3) (intro.), cr. (4), r. and recr. Table A, B, C to EM and F Register May 2009 No. 641, eff. 6-1-09; correction to Table B Parameter No. 41 made under s. 13.92 (4) (b) 7., Stats., Register September 2009 No. 645; correction to Table B Parameter No. 15 made under s. 13.92 (4) (b) 7., Stats., Register April 2010 No. 652; CR 13-112: am. (1) and (2), r. and recr. Table A, B, r. Table BM, r. and recr. Table C to F, cr. Tables G and H, Register May 2015 No. 713, eff. 6-1-15; correction in Table C footnote 11 made under s. 13.92 (4) (b) 6., Stats., Register July 2015 No. 715, eff. 8-1-15; CR 19-014: r. and recr. Table A and Notes, am. Table EM, r. and recr. Table EM Notes 8, 11, cr. Table EM Notes 16 to 23, r. and recr. Table H and Notes Register April 2020 No. 772, eff. 5-1-20; correction in (2) made under s. 35.17, Stats., Register July 2020 No. 775; CR 17-046: am. (1) Register February 2021 No. 782, eff. 6-29-21; republished to correct an error in transcription in Table F Note 1 Register January 2022 No. 793; correction in (2), Table EM Note 1 made under s. 35.17, Stats., Register June 2022 No. 798; CR 21-083: am. Table F Register July 2022 No. 799, eff. 8-1-22; correction in Table EM Note 1 made under s. 35.17, Stats., Register July 2022 No. 799.

NR 219.04 Text 1 The method must be specified when results are reported.

NR 219.04 Text 2 A 0.45-mm 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.

NR 219.04 Text 3 Microbiological Methods for Monitoring the Environment, Water, and Wastes, EPA/600/8-78/017. 1978. U.S. EPA.

NR 219.04 Text 4 U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and Analysis of Aquatic Biological and Microbiological Samples. 1989. USGS.

NR 219.04 Text 5 Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to resolve any controversies.

NR 219.04 Text 6 Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes to account for the quality, character, consistency, and anticipated organism density of the water sample.

NR 219.04 Text 7 When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of results.

NR 219.04 Text 8 To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA alternate test procedure (ATP) guidelines.

NR 219.04 Text 9 Annual Book of ASTM Standards-Water and Environmental Technology, Section 11.02. 2000, 1999, 1996. ASTM International.

NR 219.04 Text 10 Official Methods of Analysis of AOAC International. 16th Edition, 4th Revision, 1998. AOAC International.

NR 219.04 Text 11 Recommended for enumeration of target organism in sewage sludge.

NR 219.04 Text 12 The multiple-tube fermentation test is used in 9221B.2-2014. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent of all total coliform-positive tubes on a seasonal basis.

NR 219.04 Text 13 These tests are collectively known as defined enzyme substrate tests.

NR 219.04 Text 14 After prior enrichment in a presumptive medium for total coliform using 9221B.2-2014, all presumptive tubes or bottles showing any amount of gas, growth or acidity within 48 h ± 3 h of incubation shall be submitted to 9221F-2014. Commercially available EC-MUG media or EC media supplemented in the laboratory with 50 mg/mL of MUG may be used.

NR 219.04 Text 15 Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC Medium, EPA-821-R-14-009. September 2014. U.S. EPA.

NR 219.04 Text 16 Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert® may be enumerated with the multiple-well procedures, Quanti-Tray®, Quanti-Tray®/2000 and the MPN calculated from the table provided by the manufacturer.

NR 219.04 Text 17 Colilert-18® is an optimized formulation of the Colilert® for the determination of total coliforms and E. coli that provides results within 18 h of incubation at 35°C rather than the 24 h required for the Colilert® test and is recommended for marine water samples.

NR 219.04 Text 18 Descriptions of the Colilert®, Colilert-18®, Quanti-Tray®, and Quanti-Tray®/2000 may be obtained from IDEXX Laboratories, Inc.

NR 219.04 Text 19 A description of the mColiBlue24® test, is available from Hach Company.

NR 219.04 Text 20 Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium, EPA-821-R-06-013. July 2006. U.S. EPA.

NR 219.04 Text 21 Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified Membrane-Thermotolerant Escherichia coli Agar (modified mTEC), EPA-821-R-14-010. September 2014. U.S. EPA.

NR 219.04 Text 22 Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium, EPA-821-R-14-012. September 2014. U.S. EPA.

NR 219.04 Text 23 A description of the Enterolert® test may be obtained from IDEXX Laboratories Inc.

NR 219.04 Text 24 Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-b-D-Glucoside Agar (mEI), EPA-821-R-14-011. September 2014. U.S. EPA.

NR 219.04 Text 25 Standard Methods for the Examination of Water and Wastewater, Joint Editorial Board, American Public Health Association, American Water Works Association, and Water Pollution Control Federation, 23rd Edition (2017), 22nd Edition (2012), 21st Edition (2005), 20th Edition (1998), 19th Edition (1995), and 18th Edition (1992).

NR 219.04 Text 26 Standard Methods for the Analysis of Water and Wastewater. With the promulgation of Federal Register /Vol. 77, No. 97 / Friday, May 18, 2012, the EPA lists only the most recently EPA-approved version of a Standard Method (regardless of the printed or online edition) in 40 CFR Part 136, with few exceptions, to identify the method with the year of Standard Methods approval or adoption designated by the last four digits in the method number (e.g., Standard Method 3113B–2004). This approach clearly identifies the version of the standard method approved under Part 136 and no longer ties it to a particular compendium printing or edition of Standard Methods. Methods can be purchased at www.standardmethods.org.

NR 219.04 Text 27 Compliance monitoring must be performed in accordance with the specifications in the “State of Wisconsin Aquatic Life Toxicity Testing Methods Manual, 2nd Edition,” Wisconsin Department of Natural Resources, 2004. This publication is available for inspection at the offices of the Department of Natural Resources and the Legislative Reference Bureau. Copies are available from the Department of Natural Resources, Bureau of Science Services, P.O. Box 7921, Madison, WI 53707.