NR 149.02(7)(ar)
(ar) 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
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 149.02(7)(b)
(b) 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.
NR 149.02(7)(c)
(c) 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
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:
NR 149.03(1)
(1) “
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
Note:
Acceptance limits are specified in s.
NR 149.27.
NR 149.03(2)
(2) “
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.”
NR 149.03(3)
(3) “
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.
NR 149.03(4)
(4) “
Accuracy” means the closeness of a measured value to an accepted reference value or standard.
NR 149.03(5)
(5) “
Algorithm” means a process or set of rules to be followed in calculations for solving a problem.
NR 149.03(6)
(6) “
Analysis day” means the day in which a specific type of analysis is performed.
NR 149.03(7)
(7) “
Analyte” means the chemical substance, physical property, or organism analyzed in a sample.
NR 149.03(8)
(8) “
Analyte group” means a set of analytes that can be determined using the same method or tebchnology and that constitute a unit, acknowledged by the department, of the third tier of accreditation under s.
NR 149.13 (4).
NR 149.03(9)
(9) “
Analytical balance” means a balance that is capable of measuring masses to within 0.0001 g.
NR 149.03(10)
(10) “
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).
NR 149.03(11)
(11) “
Analytical instrument” means any test instrument used to provide analytical results that is not support equipment.
NR 149.03(12)
(12) “
Analytical staff” means staff that includes laboratory directors, supervisory personnel, quality assurance personnel, technicians, chemists, biologists, preparation analysts, and instrument analysts.
NR 149.03(13)
(13) “
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
Note:
Leachates are not accredited under the aqueous matrix.
NR 149.03(14)
(14) “
Batch” means a set of environmental samples prepared or analyzed together using the same process, personnel, and lots of reagents.
NR 149.03(14)(a)
(a) 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.
NR 149.03(14)(b)
(b) An “analytical batch” means a set of environmental samples which are analyzed together as a group in an uninterrupted sequence.
NR 149.03(15)
(15) “
Bias” means the consistent deviation of measured values from a true value caused by systematic errors in a procedure or a measurement process.
NR 149.03(16)
(16) “
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.
NR 149.03(17)
(17) “
Calibration blank” means an aliquot that consists of the same matrix as that used for the calibration standards, but without the analytes.
NR 149.03(18)
(18) “
Calibration function” means the specific mathematical relationship established to relate calibration standards to instrument response.
NR 149.03(19)
(19) “
Calibration model” means an algorithm that is used to determine an average calibration factor, average response factor, linear regression, or non-linear regression.
NR 149.03(20)
(20) “
Certificate” means a document owned by the department and issued to a laboratory that indicates the fields of accreditation granted to a laboratory.
NR 149.03(21)
(21) “
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.
NR 149.03(22)
(22) “
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.
NR 149.03(23)
(23) “
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.
NR 149.03(24)
(24) “
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.
NR 149.03(25)
(25) “
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.
NR 149.03(26)
(26) “
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.
NR 149.03(27)
(27) “Corrective action” means any measure taken to eliminate or prevent the recurrence of the causes of an existing nonconformity, defect, or undesirable condition.
NR 149.03(29)
(29) “
Covered program” means a program listed or enumerated in s.
299.11 (1) (d) 1. to
9., 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
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.
NR 149.03(30)
(30) “
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.
NR 149.03(31)
(31) “
Department” means the department of natural resources.
NR 149.03(32)
(32) “
EPA” means the United States environmental protection agency.
NR 149.03(33)
(33)
“Field of accreditation” means a 3-tiered unit by which the department uses to grant laboratories accreditation as specified under s.
NR 149.13.
NR 149.03(34)
(34) “
For hire” means offering analyses for payment or non-monetary compensation.
NR 149.03(35)
(35) “
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.
NR 149.03(36)
(36) “
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.
NR 149.03(37)
(37) “
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.
NR 149.03(38)
(38) “
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.
NR 149.03(39)
(39) “
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
Note:
In many EPA methods, the term “lab-fortified blank” is equivalent to an LCS.
NR 149.03(40)
(40) “
Laboratory equipment” means any support equipment or analytical instrument necessary to or involved in generating the results of an analysis.
NR 149.03(41)
(41) “
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).
NR 149.03(42)
(42) “
Limit of quantitation” or “LOQ” means the lowest concentration or amount of an analyte for which quantitative results can be obtained.
NR 149.03(43)
(43) “
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.
NR 149.03(44)
(44) “
Method” means a procedure used for measuring the presence and concentration of physical and chemical pollutants.
NR 149.03(45)
(45) “
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
Note:
In many EPA methods, the term “laboratory reagent blank” is equivalent to a method blank.
NR 149.03(46)
(46) “
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
Note:
Links to
40 CFR Part 136, Appendix B can be found on the Wisconsin department of natural resources laboratory accreditation program website.
NR 149.03(47)
(47) “
NIST” means the National Institute for Standards and Technology.
NR 149.03(48)
(48) “
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.
NR 149.03(49)
(49) “
Nonconformance” means a documented or verifiable deviation from the requirements of this chapter or a deviation from the requirements of a quality system.
NR 149.03(50)
(50) “
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.
NR 149.03(51)
(51) “
Ownership” means owning or controlling, directly or indirectly, a laboratory facility through an equity interest, or its equivalent, of 10% or more.
NR 149.03(52)
(52) “
Pesticide” means a chemical substance defined in s.
94.67 (25) and
(25m), Stats., an isomer of a pesticide or a degradation product or metabolic product of a pesticide.
NR 149.03(53)
(53) “
Precision” means the degree to which a set of observations or measurements of the same property, obtained under similar conditions, conform to themselves. Precision is usually expressed as the standard deviation, variance, or range, in either absolute or relative terms.
NR 149.03(54)
(54) “
Proficiency testing sample” or “PT sample” means a sample obtained from an approved proficiency testing sample provider to evaluate the ability of a laboratory to produce an analytical test result meeting the definition of acceptable performance outlined in s.
NR 149.27. The concentration of the analyte in the sample is unknown to the laboratory at the time of analysis.
NR 149.03(55)
(55) “
Qualify” means a written statement accompanying or referencing test results to identify anomalies or deviations from the requirements in this chapter that were encountered in generating the results.
NR 149.03(56)
(56) “
Quality assurance” means an integrated system of activities involving planning, control, assessment, reporting, and improvement to ensure that a product or service meets defined standards of quality.
NR 149.03(57)
(57) “
Quality control” means the overall system of technical activities designed to measure and control the quality of a product or service that meets the stated needs of users.
NR 149.03(58)
(58) “
Quality control limit” means the acceptance criteria used to evaluate quality control samples. Quality control limits may be those published by the department, referenced in a method or calculated by a laboratory. In this chapter, quality control limits calculated by a laboratory will be referred to as generated in-house control limits.
NR 149.03(59)
(59) “
Quality system” means a structured and documented management arrangement describing the policies, objectives, principles, organizational authority, responsibilities, accountability, and implementation plan of an organization for ensuring quality in its work processes, products, and services.
NR 149.03(60)
(60) “
Raw data” means any original information from a measurement activity or study recorded in media that allows the reconstruction and evaluation of the activity or study. “Raw data” include absorbance, emission counts, area counts, peak heights, abundance, and millivolts. Raw data may be stored in hard copy or electronically.
NR 149.03(61)
(61) “
Reagent water” means water which has been treated to remove any impurities that may affect the quality of an analysis.
NR 149.03(62)
(62) “
Reference material” means a material that has one or more sufficiently well-established properties that can be used for calibrating or verifying the calibration of support equipment or analytical instruments.
NR 149.03(63)
(63) “
Registration” or “registered” means registration under s.
299.11 (8), Stats., of laboratories that perform tests solely on its own behalf or that of a subsidiary under common ownership or control in accordance with the standards and requirements of this chapter. Registered laboratories do not perform drinking water testing.
NR 149.03(64)
(64) “
Relative standard error” or “RSE” means the standard error divided by the mean for a set of calibration data and expressed as a percentage. The RSE is calculated according to the following formula:
xi = true amount of analyte in calibration level
i, in mass or concentration units.
x‵i = measured amount of analyte in calibration level i, in mass or concentration units.
p = number of terms in the fitting equation.
NR 149.03 Note
Note:
average = 1, linear = 2, quadratic = 3, cubic = 4
n = number of calibration points.
NR 149.03(66)
(66) “
Relocation” means a move by a laboratory resulting in a change in the laboratory's physical address.
NR 149.03(67)
(67) “
Replicate” means two or more substantially equal aliquots analyzed independently for the same analyte.
NR 149.03(68)
(68) “
Residual” means the difference, expressed as a percent, between the theoretical concentration of a calibration standard and the value derived from the calibration function from the measured response of the calibration standard.
