NR 149.39(2)(b) (b) Certificates issued to the laboratory by entities with which the department has entered into a reciprocal agreement under s. NR 149.08, if a laboratory is accredited for this chapter under any existing agreement.
NR 149.39(2)(c) (c) Records of personnel qualifications, experience, and training when personnel are required to possess or maintain specific credentials by s. NR 149.36 (2).
NR 149.39(2)(d) (d) Copies of, or access to, other regulations, standards, and documents necessary for the laboratory to operate or to maintain compliance with this chapter.
NR 149.39(3) (3)Reagent and standard records and reference materials. The laboratory shall document the identity, source, and purity of standards and reagents used in the methods performed. The laboratory shall retain records of reference materials and certificates of analysis when the records are provided by the supplier and are necessary to establish the identity, source, or purity of standards and reagents.
NR 149.39(3)(a) (a) Reagent containers shall be labeled with an expiration date, chemical name, and concentration. Except for instrument vials, standard containers shall be labeled with an expiration date, chemical name, and concentration.
NR 149.39(3)(b) (b) The laboratory shall document the lot number, manufacturer, chemical name, concentration, and the date of expiration for standards and reagents purchased from a manufacturer. These records shall be separate from the container labels.
NR 149.39 Note Note: An expiration date is not required when one is not provided by the supplier.
NR 149.39(3)(c) (c) The laboratory shall document the preparation details of all prepared standards and reagents. These records shall link the prepared standards and reagents to the respective originating stocks or neat compounds and shall indicate the date of preparation, date of expiration, and the identity of the preparer.
NR 149.39(3)(d) (d) The laboratory may not use any standards and reagents beyond the expiration dates unless the laboratory is using the standard and reagents for qualitative determinations.
NR 149.39(3)(e) (e) Certificates for all reference materials shall be maintained.
NR 149.39(4) (4)Analytical and technical records. The format of the analytical and technical records of a laboratory shall facilitate access to the information in this subsection and may be contained in bench sheets, log books, notebooks, journals, manuals, standard operating procedures under s. NR 149.40, and forms, in hard copy or electronic media.
NR 149.39(5) (5)Sample collection records. The laboratory shall retain records supplied by the collector to allow the laboratory to evaluate collection information against the laboratory's sample acceptance policy.
NR 149.39 History History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21.
NR 149.40 NR 149.40 Standard operating procedures.
NR 149.40(1)(1)A laboratory shall maintain written standard operating procedures that document or reference activities needed to maintain its quality systems and that enable performing or reproducing an analysis in its entirety as performed at the laboratory. Each laboratory shall develop, maintain, and keep current its standard operating procedures for both sample preparation and analysis.
NR 149.40 Note Note: Sample preparation includes digestions, distillations, extractions, concentrations, dilutions, and clean-up performed on samples prior to the determinative analytical step.
NR 149.40(2) (2) Standard operating procedures may be documents written by laboratory personnel or may consist entirely of copies of published documents, manuals, or procedures if the laboratory follows the chosen source exactly.
NR 149.40(3) (3) Standard operating procedures may consist, in part, of copies of published documents, manuals, or procedures if all the following conditions are met:
NR 149.40(3)(a) (a) Modifications to the published source are described in writing in additional documents.
NR 149.40(3)(b) (b) Clarifications, changes, or choices are completely described in additional documents, when published sources offer multiple options, ambiguous directives, or insufficient detail to perform or reproduce an analysis.
NR 149.40(4) (4) Standard operating procedures shall indicate the dates of issue or revision.
NR 149.40(5) (5) When the standard operating procedure is written by the laboratory, each standard operating procedure shall include, address, or refer to all the following elements, if applicable:
NR 149.40(5)(a) (a) Identification of the referenced method.
NR 149.40(5)(b) (b) For multi-analyte methods, a list of analytes.
NR 149.40(5)(c) (c) Potential interferences and how the interferences are treated.
NR 149.40(5)(d) (d) Equipment and analytical instruments.
NR 149.40(5)(e) (e) Consumable supplies, reagents, and standards.
NR 149.40(5)(f) (f) Sample preservation, storage, and hold time.
NR 149.40(5)(g) (g) Quality control samples and frequency of the analysis.
NR 149.40(5)(h) (h) Calibration and standardization.
NR 149.40(5)(i) (i) Procedure for analysis.
NR 149.40(5)(j) (j) Data assessment and acceptance criteria for quality control measures.
NR 149.40(5)(k) (k) Corrective actions and contingencies for handling out of control or unacceptable data.
NR 149.40 History History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21.
NR 149.41 NR 149.41 Method selection.
NR 149.41(1)(1)The laboratory shall use methods for environmental testing required by covered programs under this chapter and that are suitable for the matrix, type of analyte, expected level of analyte, regulatory limit, and potential interferences in the samples to be tested.
NR 149.41 Note Note: Sources, including the following as updated, likely contain methods that are acceptable for testing under this chapter: The EPA, the department, Standard Methods for the Examination of Water and Wastewater, Test Methods for Evaluating Solid Waste, Physical/Chemical Methods – SW-846, American Society for Testing and Materials, and the U.S. Geological Survey Agency.
NR 149.41(2) (2) When methods are not specified by covered programs under this chapter or specified in permits issued by the department, the laboratory shall consult with the department to select a method that meets the requirements in sub. (1).
NR 149.41(3) (3) When using methods associated with the methods compendium document, “Test Methods for Evaluating Solid Waste,” the laboratory shall comply with the minimum requirements of the methods as written and state which options are being implemented when options exist.
NR 149.41 Note Note: The documents above can be found on the Wisconsin department of natural resources laboratory accreditation program website and are available for inspection at the offices of the department and the legislative reference bureau.
NR 149.41(4) (4) The department will assess the scientific validity of method modifications to determine if the modification is within the scope of a method.
NR 149.41 History History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21.
NR 149.42 NR 149.42 Alternative methods.
NR 149.42(1)(1)The department may allow the use of alternative methods from those required by covered programs, including the safe drinking water program, if a laboratory requests approval and if the EPA has granted approval for the alternative methods.
NR 149.42(2) (2) On a case-by-case basis, the department may allow the use of methods other than those required by covered programs for any of the following situations:
NR 149.42(2)(a) (a) After consultation with the department, the manager of a covered program determines that the allowance does not result in a detrimental effect on the quality and defensibility of the results to be generated.
NR 149.42(2)(b) (b) The request is for approval of a method that employs a new or emerging technology and there is documentation that substantiates the validity of the new or emerging technology for the intended purpose.
NR 149.42(3) (3) Requests to use an alternative method shall include the reason for seeking the approval, a description of the principles of any new or emerging technology involved, and the potential scope of application of the method. The department may establish criteria for validating the method for the specific application and scope requested. If the laboratory's method validation results meet the established validation criteria, the department shall allow the use of the method for the specific application and scope requested.
NR 149.42(4) (4) The department shall approve or deny the request for consideration of approval for use within 90 days from the receipt of the request. The department shall consider in its decision whether the covered programs that would be the recipients of the data generated have a demonstrated need for allowing the alternative method.
NR 149.42(5) (5) The department may charge a fee under s. 299.11 (5) (d), Stats., if it is necessary to verify the results of any validation data submitted by a laboratory requesting use of an alternative method.
NR 149.42 History History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21.
NR 149.43 NR 149.43 Laboratory facilities.
NR 149.43(1)(ag) (ag) The laboratory shall ensure that the environmental conditions of its facility do not adversely affect the required quality of any measurement.
NR 149.43(1)(ar) (ar) Laboratory facilities shall ensure effective separation between neighboring areas in which incompatible analytical activities take place. The laboratory shall take measures to prevent cross-contamination.
NR 149.43(1)(b) (b) Access to and use of areas affecting the quality of environmental tests shall be controlled to an extent commensurate with the type of analysis and samples analyzed by a laboratory.
NR 149.43(2) (2) The laboratory shall monitor, control, and record environmental conditions when the environmental conditions are required by the methods or when the environmental conditions influence the quality of test results.
NR 149.43 History History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21; renum. (1) (intro.), (a) to (1) (ag), (ar) under s. 13.92 (4) (b) 1., Stats., Register February 2021 No. 782.
NR 149.44 NR 149.44 Laboratory equipment.
NR 149.44(1)(1)General provisions.
NR 149.44(1)(a)(a) The laboratory shall furnish the equipment necessary and required for the correct performance of all the environmental tests and associated preparations and activities it performs.
NR 149.44(1)(b) (b) The laboratory shall use equipment and software for testing and calibration that achieves the accuracy required to comply with the requirements of the methods or specifications relevant to the environmental testing performed by the laboratory.
NR 149.44(2) (2)Laboratory support equipment.
NR 149.44(2)(a) (a) The laboratory shall use support equipment only for its intended purpose, and it shall keep that equipment in working order by routine and preventive maintenance.
NR 149.44(2)(b) (b) When support equipment leaves the direct control of the laboratory for maintenance or for any other reason, the laboratory shall ensure that the function and calibration status of that equipment is checked or demonstrated to be in working order before the equipment is returned to service.
NR 149.44(3) (3)Calibration and verification of support equipment.
NR 149.44(3)(a)(a) The laboratory shall calibrate or verify all support equipment within that equipment's range of use using available reference materials traceable to NIST. When reference materials traceable to NIST are not commercially available, the laboratory shall use materials of a quality that will ensure the accuracy of the calibrated or verified support equipment for its intended use.
NR 149.44(3)(b) (b) The acceptability criteria for these calibration or verification checks shall be established by the methods, or in the absence, department guidance.
NR 149.44 Note Note: Department guidance can be found on the Wisconsin department of natural resources laboratory accreditation program website.
NR 149.44(3)(c) (c) The laboratory shall establish a procedure for calibrating or verifying the calibration of support equipment which shall include all the following elements:
NR 149.44(3)(c)1. 1. Procedures used for calibrating or verifying the calibration.
NR 149.44(3)(c)2. 2. Procedures for utilization of correction factors when there is a bias.
NR 149.44(3)(c)3. 3. Evaluation criteria used which defensibly documents the continued accuracy of the equipment.
NR 149.44(3)(c)4. 4. Procedures for addressing equipment which fails to meet calibration or verification requirements.
NR 149.44(3)(d) (d) Minimum verification frequencies include all the following:
NR 149.44(3)(d)1. 1. Annually: devices used to measure atmospheric pressure and temperature.
NR 149.44(3)(d)2. 2. Quarterly: mechanical and automatic volumetric dispensing devices, including pipettes.
NR 149.44(3)(d)3. 3. Monthly: balances, with one weight in the expected range of use. Balance weights shall be all the following:
NR 149.44(3)(d)3.a. a. Handled and stored in a manner that protects the weights' integrity.
NR 149.44(3)(d)3.b. b. Traceable to NIST and of class 2 quality or better. Certified for accuracy every five years by a metrology service outside the laboratory. Alternatively, new weights of class 2 quality or better, traceable to NIST, shall be purchased for use. Weight recertification shall be performed sooner than every five years if balance checks performed using these weights suggest that a change in the certified weights has occurred.
NR 149.44 Note Note: Weights that are currently NIST traceable may be used to verify other weights.
NR 149.44(3)(d)4. 4. Each day of use: when specific temperatures are required by method, regulation, or covered program, the operating temperature of the equipment used to control temperatures shall be checked and documented.
NR 149.44(3)(e) (e) All the following are exempt from accuracy verification under this section:
NR 149.44(3)(e)1. 1. Glass microliter syringes.
NR 149.44(3)(e)2. 2. Disposable pipettes.
NR 149.44(3)(e)3. 3. Automatic titrator systems.
NR 149.44(4) (4)Laboratory analytical instruments.
NR 149.44(4)(a) (a) The laboratory shall use personnel properly trained to operate analytical instruments. Instructions on the use and maintenance of equipment shall be available to instrument operators.
NR 149.44(4)(b) (b) The laboratory shall properly maintain, inspect, and clean all instruments. The laboratory shall establish procedures for the maintenance of analytical instruments to prevent contamination or deterioration that may affect reported results.
Published under s. 35.93, Stats. Updated on the first day of each month. Entire code is always current. The Register date on each page is the date the chapter was last published.