Quality control requirements for chemical testing.
Ch. NR 149 Note
Chapter NR 149 as it existed on April 30, 2008, was repealed and a new chapter NR 149 was created, Register April 2008 No. 628
, effective September 1, 2008. Chapter NR 149 as it existed on June 28, 2021, was repealed and a new chapter NR 149 was created, Register February 2021 No. 782, effective June 29, 2021.
NR 149.01 Purpose.
The purpose of this chapter is to establish a program for the accreditation of laboratories performing testing under s. 299.11
NR 149.01 History
History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21. NR 149.02(1)(1)
This chapter specifies requirements for the administration of the laboratory accreditation program by the department.
Unless otherwise exempted in this section, this chapter applies to all the following:
Laboratories submitting data to the department for a covered program.
Laboratories generating data that is necessary for the department to determine compliance with a covered program.
NR 149.02 Note
Administrative codes and covered programs requiring analyses to be performed by an accredited laboratory are chs. NR 101
– Reports And Fees For Wastewater Discharges, 102 – Water Quality Standards For Wisconsin Surface Waters, 106 – Procedures For Calculating Water Quality Based Effluent Limitations For Point Source Discharges To Surface Waters, 110 – Sewerage Systems, 123 – Well Compensation Program, 131 – Nonferrous Metallic Mineral Prospecting, 132 – Nonferrous Metallic Mineral Mining, 140 – Groundwater Quality, 150 – Environmental Analysis And Review Procedures, 153 – Targeted Runoff Management And Notice Of Discharge Grant Programs, 155 – Urban Nonpoint Source Water Pollution Abatement And Storm Water Management Grant Program, 157 – Management Of Pcbs And Products Containing Pcbs, 182 – Nonferrous Metallic Mineral Mining Wastes, 200 – Application For Discharge Permits And Water Quality Standards Variances, 204 – Domestic Sewage Sludge Management, 205 – General Provisions, 206 – Land Disposal Of Municipal And Domestic Wastewaters, 210 – Sewage Treatment Works, 211 – General Pretreatment Requirements, 212 – Waste Load Allocated Water Quality Related Effluent Limitations, 214 – Land Treatment Of Industrial Liquid Wastes, By-Product Solids And Sludges, 216 – Storm Water Discharge Permits, 217 – Effluent Standards And Limitations For Phosphorus, 218 – Method And Manner Of Sampling, 219 – Analytical Test Methods And Procedures, 230 – Inorganic Chemicals Manufacturing, 233 – Pesticide Chemicals, 243 – Animal Feeding Operations, 254 – Iron And Steel Manufacturing, 256 – Metal Molding And Casting, 260 – Electroplating, 261 – Metal Finishing, 263 – Coil Coating, 273 – Nonferrous Metals Forming And Metal Powders, 274 – Nonferrous Metals Manufacturing, 290 – Steam Electric Power Generating, 347 – Sediment Sampling And Analysis, Monitoring Protocol And Disposal Criteria For Dredging Projects,
500 – General Solid Waste Management Requirements, 507 – Environmental Monitoring For Landfills, 518 – Landspreading Of Solid Waste, 528 – Management Of Accumulated Sediment From Storm Water Management Structures,
538 – Beneficial Use Of Industrial Byproducts, 662 – Hazardous Waste Generator Standards, 664 – Hazardous Waste Treatment, Storage And Disposal Facility Standards, 665 – Interim License Hazardous Waste Treatment, Storage And Disposal Facility Standards, 700 – General Requirements, 712 – Personnel Qualifications For Conducting Environmental Response Actions, 716 – Site Investigations,
720 – Soil Cleanup Standards, 738 – Temporary Emergency Water Supplies, 747 – Petroleum Environmental Cleanup Fund, 809 – Safe Drinking Water, 810 – Requirements For The Operation And Maintenance Of Public Water Systems, 811 – Requirements For The Operation And Design Of Community Water Systems, 812 – Well Construction And Pump Installation and 845 – County Administration Of NR 812 Private Wells Code.
NR 149.02 Note
Links to the codes specified above can be found on the Wisconsin department of natural resources laboratory accreditation program website.
Laboratories performing analyses for the safe drinking water program under ch. NR 809
or for the well construction and pump installation testing program under ch. NR 812
shall be certified; registration is not available for these analyses. Additional requirements for laboratories performing compliance analysis under ch. NR 809
are specified in s. NR 149.19
Laboratories performing analysis for whole effluent toxicity testing shall meet the requirements specified in s. NR 149.20
This chapter applies to laboratories analyzing industrial pre-treatment samples when the department is the control authority of a pre-treatment ordinance or when another control authority requires it.
Laboratories performing asbestos or radiological testing for a covered program shall be certified or approved by the EPA or the department.
NR 149.02 Note
Laboratories performing bacteriological testing for a covered program are certified or approved under ch. ATCP 77
by the department of agriculture, trade, and consumer protection.
This chapter establishes compliance requirements that shall be incorporated into the quality systems of all laboratories accredited by the department.
Laboratories shall meet any requirements pertaining to analyses and analytical operations contained in the methods, regulations, or covered programs when those requirements are more stringent than the ones specified in this chapter, unless this chapter grants explicit, alternative allowances.
NR 149.02 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.
When it is not apparent to the laboratory whether the minimum requirements of this chapter or those specified in the methods, regulations, or covered programs are more stringent, the department shall communicate which requirements are more stringent to the laboratories and the laboratories shall meet those requirements.
When a laboratory incorporates a procedure that is neither expressly permitted nor prohibited by the method, the department will assess the scientific validity of the procedure to determine if the procedure is within the scope of the method. The underlying chemistry of the method shall remain unchanged. The department may seek the advice of the council in making determinations under this paragraph.
NR 149.02 Note
For example, if a digestion time of 30 minutes is required, the laboratory is not to use less time for digestion. A second example, when a minimum volume of solvent is required to extract a specific amount of sample, then less solvent is not to be used unless the ratio of extraction solvent to sample amount is maintained.
NR 149.02 History
History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21; renum. (7) (intro.), (a) to (7) (ag), (ar) under s. 13.92 (4) (b) 1., Stats., Register February 2021 No. 782. NR 149.03
NR 149.03 Definitions.
In this chapter:
Acceptance limits” means limits established by the department that are used to determine if a laboratory has analyzed a proficiency testing sample successfully.
NR 149.03 Note
Acceptance limits are specified in s. NR 149.27
Accreditation” and “accredited” mean that the department has determined that an organization is competent to perform specific types of tests. “Accreditation” and “accredited” include “certification” and “registration.”
Accreditation matrix” means a matrix type that is part of the first tier of a field of accreditation under s. NR 149.13 (2)
. Accreditation matrices are drinking water, aqueous, and non-aqueous matrices.
Accuracy” means the closeness of a measured value to an accepted reference value or standard.
Algorithm” means a process or set of rules to be followed in calculations for solving a problem.
Analysis day” means the day in which a specific type of analysis is performed.
Analyte” means the chemical substance, physical property, or organism analyzed in a sample.
Analyte group” means a set of analytes that can be determined using the same method or technology and that constitute a unit, acknowledged by the department, of the third tier of accreditation under s. NR 149.13 (4)
Analytical balance” means a balance that is capable of measuring masses to within 0.0001 g.
“Analytical class” means a set of analytes or analyte groups of similar behavior or composition, or a set of analytes or analyte groups regulated under the same provisions of the federal safe drinking water act, that is used to organize the third tier of accreditation under s. NR 149.13 (4)
“Analytical instrument” means any test instrument used to provide analytical results that is not support equipment.
“Analytical staff” means staff that includes laboratory directors, supervisory personnel, quality assurance personnel, technicians, chemists, biologists, preparation analysts, and instrument analysts.
“Aqueous” means an accreditation matrix that is water, is not drinking water, and can be reported in units of mass per volume.
NR 149.03 Note
Leachates are not accredited under the aqueous matrix.
“Batch” means a set of environmental samples prepared or analyzed together using the same process, personnel, and lots of reagents.
A “preparation batch” means a set of one to 20 environmental samples of the same accreditation matrix, meeting batch criteria, and with a maximum time of 24 hours between the start of processing of the first and last sample in the batch.
An “analytical batch” means a set of environmental samples which are analyzed together as a group in an uninterrupted sequence.
“Bias” means the consistent deviation of measured values from a true value caused by systematic errors in a procedure or a measurement process.
“Calibration” means the process used to establish an observed relationship between the response of an analytical instrument and a known amount of analyte, or the process used to determine, by measuring or comparison with a reference standard, the correct value of each scale reading in an instrument, meter, or measuring device.
“Calibration blank” means an aliquot that consists of the same matrix as that used for the calibration standards, but without the analytes.
“Calibration function” means the specific mathematical relationship established to relate calibration standards to instrument response.
“Calibration model” means an algorithm that is used to determine an average calibration factor, average response factor, linear regression, or non-linear regression.
“Certificate” means a document owned by the department and issued to a laboratory that indicates the fields of accreditation granted to a laboratory.
“Certification” or “certified” means certification, under s. 299.11 (7)
, Stats., of laboratories that perform compliance analyses for hire or to laboratories that perform compliance drinking water analyses in accordance with the standards and requirements of this chapter.
“Coefficient of determination” means a quantity that measures the degree of agreement between the points in a calibration and the function derived to connect the points.
“Confirm” means to verify the identity of a compound by an alternative procedure, column, detector, wavelength, or by a technology that bases detection on a different scientific principle from the one originally used for identifying the compound.
“Continuing calibration blank” or “CCB” means an aliquot that consists of the same matrix as that used for the calibration standards, but without the analytes, analyzed during an analysis sequence to verify the continued absence of instrumental interferences.
“Continuing calibration verification standard” or “CCV standard” means a standard of known concentration of analyte used to assure continued calibration accuracy during an analysis sequence.
“Correlation coefficient” means a quantity that measures the degree of agreement between the points in a calibration curve and the linear function derived to connect the points.
“Corrective action” means any measure taken to eliminate or prevent the recurrence of the causes of an existing nonconformity, defect, or undesirable condition.
“Covered program” means a program listed or enumerated in s. 299.11 (1) (d) 1.
, Stats., and includes any department program, project, permit, contract, or site investigation that requires analytical work to be performed by an accredited laboratory.
NR 149.03 Note
The note in s. NR 149.02 (2) (d)
provides a list of department administrative rules of covered programs requiring accreditation under this chapter.
“Deficiency” means a documented or verifiable deviation from the requirements of this chapter that is noted during an on-site evaluation or while reviewing analytical data produced by a laboratory.
“Department” means the department of natural resources.
“EPA” means the United States environmental protection agency.
“Field of accreditation” means a 3-tiered unit by which the department uses to grant laboratories accreditation as specified under s. NR 149.13
“For hire” means offering analyses for payment or non-monetary compensation.
“Initial calibration blank” or “ICB” means an aliquot that consists of the same matrix as that used for the calibration standards, but without the analytes, analyzed following the initial calibration and prior to quantitating any samples to verify the absence of instrumental interferences.
“Initial calibration verification standard” or “ICV standard” means a standard of known concentration, prepared using second source standards, analyzed following the initial calibration and prior to quantitating any samples to assure initial calibration accuracy.
“Internal standard” means a known concentration of standard added to a sample or quality control sample as a reference for evaluating and controlling the precision and bias of the analytical method.
“Laboratory” means a facility that performs tests in connection with a covered program that requires data from an accredited laboratory. A facility consisting of a principal laboratory and annexes within 5 miles of the principal laboratory may be considered a single laboratory. When the terms “laboratory” or “laboratories” are used unmodified in this chapter, the terms include laboratories accredited under this chapter and those seeking accreditation under this chapter.
“Laboratory control sample” or “LCS” means a sample of a matrix without the analytes of interest or a matrix with a consistent concentration of the analytes of interest, fortified with a verified known amount of the analytes of interest. The purpose of an LCS is to determine whether the methodology is in control and whether the laboratory can make accurate and precise measurements.
NR 149.03 Note
In many EPA methods, the term “lab-fortified blank” is equivalent to an LCS.
“Laboratory equipment” means any support equipment or analytical instrument necessary to or involved in generating the results of an analysis.
“Limit of detection” or “LOD” means the lowest concentration or amount of analyte that can be identified, measured, and reported with confidence that the concentration is not a false positive value. The department considers the LOD to be equivalent to the method detection limit and is determined under the method cited in sub. (46)
“Limit of quantitation” or “LOQ” means the lowest concentration or amount of an analyte for which quantitative results can be obtained.
“Maximum contaminant level” or “MCL” means the maximum permissible level of a contaminant in water that is delivered to any user of a public water system.
“Method” means a procedure used for measuring the presence and concentration of physical and chemical pollutants.
“Method blank” means a clean matrix that is treated and processed exactly as a sample including exposure to all glassware, equipment, solvents, reagents, internal standards, and surrogates to measure artifacts in the measurement process.
NR 149.03 Note
In many EPA methods, the term “laboratory reagent blank” is equivalent to a method blank.
“Method detection limit” or “MDL” means the minimum measured concentration of a substance that can be reported with 99% confidence that the measured concentration is distinguishable from method blank results. The MDL is generated according to the procedure specified in the latest revision of 40 CFR Part 136
, Appendix B.
NR 149.03 Note
Links to 40 CFR Part 136
, Appendix B can be found on the Wisconsin department of natural resources laboratory accreditation program website.
“NIST” means the National Institute for Standards and Technology.
“Non-aqueous” includes all matrices that are not drinking water or aqueous. It includes soils, sediments, sludges, organic liquids, oils, solid waste, and multi-phasic wastes. Leachates are accredited under the non-aqueous matrix.
“Nonconformance” means a documented or verifiable deviation from the requirements of this chapter or a deviation from the requirements of a quality system.
“On-site evaluation” means an assessment conducted by the department at a laboratory seeking or maintaining accreditations to determine actual or potential compliance with the requirements of this chapter.
“Ownership” means owning or controlling, directly or indirectly, a laboratory facility through an equity interest, or its equivalent, of 10% or more.