When an initial instrument calibration is not performed on the day of analysis, the continuing validity of the initial calibration shall be verified prior to analyzing any batch quality control or environmental samples by the analysis of one or more CCV standards, subject to all the following:
Except for multi-peak analytes, CCV standards shall contain all analytes to be reported and may be prepared from the same standards used to generate the initial calibration. CCV standards are required for multi-peak analytes when the analytes are detected and reported in the samples.
CCV standards shall be treated the same as the standards used in the initial calibration. When the method requires that the standards be treated the same as samples, the CCV standards shall be performed with the associated batch so that the CCV standards and samples are all processed together.
Continuing calibration verification is not required for technologies when there are no initial calibrations established.
If an LCS also serves as a CCV standard, the acceptance criteria of the CCV standard shall be used.
Continuing calibration verification shall be performed at least once on each analysis day when an initial calibration is not performed and prior to sample analysis and batch quality control analysis.
Continuing calibration verification shall be performed after the consecutive analysis of each group of 20 environmental samples, if 20 or more samples constitute an analytical batch, unless otherwise required by method, regulation, or covered program.
Minimum number of standards and concentration levels. NR 149.446(3)(a)(a)
For linear and quadratic model calibration functions, the laboratory shall analyze at least a single CCV standard. The concentration of the standard shall be within the range established during the initial calibration.
NR 149.446 Note
Linear calibration models include electrometric technologies (pH and ion selective electrode), average response factor, average calibration factor, linear regression, and least squares analysis.
For cubic model calibration functions or third order polynomials, the laboratory shall analyze at least two CCV standards in each instance when a single CCV standard is required by method, regulation, or covered program.
Unless otherwise required by method, regulation, or covered program, the acceptance criteria for CCV standards shall be within 10% of the theoretical concentrations of all reportable inorganic analytes from an initial calibration.
Unless otherwise required by method, regulation, or covered program, the acceptance criteria for CCV standards shall be within 20% of the theoretical concentrations of all reportable organic analytes from an initial calibration.
When a CCV standard fails, the laboratory shall do any of the following:
Perform corrective action and reanalyze the CCV standard. If the CCV standard does not pass, an initial calibration shall be performed.
Perform a second consecutive (immediate) CCV standard under the same conditions. If the second CCV standard also fails, then corrective action shall be performed and two consecutive CCV standards shall pass or an initial calibration shall be performed.
When the method requires that the standards be treated the same as the samples and when the method requires a CCB, the CCB shall be performed with the associated batch so that the CCB and samples are all processed together. The CCB is processed at the same frequency as the CCV standard. The CCB is subject to the same criteria specified in s. NR 149.48 (5) (d)
NR 149.446 History
History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21. NR 149.45
The laboratory shall maintain all analytical and technical records containing raw and derived data or original observations necessary to allow historical reconstruction of all laboratory activities that contributed to generating reported results. Observations, data, and calculations shall be recorded at the time they are made. At a minimum, the laboratory shall ensure that results of analyses can be linked to sample collection data, preparation records, calibration records, analytical records, test reports, corrective action, and any chemicals used.
NR 149.45 History
History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21. NR 149.47(1)(a)(a)
The laboratory shall report results of each test performed by the laboratory in accordance with any requirements or instructions specified in the methods or by the department.
The laboratory shall quantitate sample results only from initial instrument calibrations, unless otherwise allowed by method, regulation, or covered program or unless any of the following applies:
Samples analyzed by inductively coupled plasma emission spectrophotometers and inductively coupled plasma mass spectrometers having responses at or greater than 90% of the established upper limit of the linear dynamic range of the instruments shall be diluted and reanalyzed.
When an analyte does not perform as well as most of the analytes in a multi-analyte initial calibration, analysis may proceed, and results reported for these analytes, provided that the results are appropriately qualified as required in this section.
When samples cannot be diluted and reanalyzed, the laboratory shall report sample results with appropriate qualifiers.
The laboratory shall establish procedures for reporting results for samples analyzed by dual column and dual detector systems. These procedures shall establish all the following prior to analysis:
A primary column or primary detector from which results shall be reported.
The conditions under which a presumptive identification is confirmed and reported from the secondary column or detector.
When results are greater than the LOQ on dual column or dual detector systems, and the RPD exceeds 40%, then the higher of the two results shall be reported unless the analyst defensibly documents that the higher result is biased due to interference. In this case the laboratory may report the lower result with a qualifier indicating the value of the higher result or report both results.
Excluding microbiological results, MCL exceedances for any regulated analyte associated with ch. NR 809
compliance monitoring shall be reported by the laboratory to the affected water supply facility within 48 hours of completing sample results.
NR 149.47 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.
Laboratory test reports shall have formats that facilitate reviewing the content elements specified in this section, unless otherwise provided by pars. (b)
, and (d)
. Content elements may be presented in any form, including electronic media.
When tests are performed for internal clients or when a laboratory has a written agreement with a client, the laboratory may issue reports without all the content elements specified in this section. The laboratory shall retain and make available to the department, upon request, records that include the content elements specified in this section.
A laboratory that is operated by a facility whose function is to provide data to monitor the facility's compliance with covered programs shall retain and make available to the department, upon request, records that include the content elements specified in this section. Laboratory reports with all the content elements specified in this section are not required to be issued if any of the following apply:
The laboratory is responsible for preparing regulatory reports in a specified format to the department.
The laboratory provides information to another individual within the facility for preparation of regulatory reports in a specified format to the department.
Unless otherwise specified by the department, for covered programs that receive data on behalf of a facility, directly from a laboratory, or when provided by pars. (b)
, test reports from the laboratory shall include all the following information.
The sample identifying information provided by the client or collector.
Identification of the methods used for preparation and analysis.
Collection, preparation, and analysis times for tests with holding times expressed in hours.
The dates of analysis, extraction, or digestion, when a holding time has been established for the preparation step.
When non-aqueous sample results are reported, the laboratory shall indicate whether the non-aqueous sample results were reported on a dry weight or wet weight basis.
The LOD and LOQ for tests which the department requires reporting to the LOD.
Except for HRGC/MS analysis, for sample results requiring adjustments, an indication of whether the LOD and LOQ have been adjusted accordingly.
NR 149.47 Note
Sample adjustments are any sample dilutions or sample amounts that were used differently than those used in the initial demonstration of capability and MDL studies.
The identity of the subcontract laboratory, for each reported result generated by a subcontract laboratory.
A laboratory may make amendments to a test report already issued by the laboratory in a manner that clearly identifies the reasons for the amendment and that references the original laboratory test report.
Amended reports shall comply with the requirements of this section.
Sample rejection or qualification of results.
The laboratory shall handle results for samples received with insufficient volume to complete the requested analyses, samples received beyond holding time, samples received improperly preserved, samples received in inappropriate containers, or samples received showing evidence that the samples have not been collected according to approved procedures as follows:
Drinking water samples shall be rejected for analysis unless the laboratory has documented instructions from the client to proceed with analyses and all reported results are accompanied by a disclaimer attesting that the results may not be used to determine or evaluate compliance with the safe drinking water act.
Non-drinking water samples shall be rejected for analysis or appropriately qualified.
Samples requiring reanalysis or qualification of results.
Samples shall be re-analyzed, or the affected sample results qualified when any of the following occur:
The concentration of an analyte in the ICB exceeds its LOD.
Surrogates or internal standard recoveries exceed limits, unless the failures result from matrix interference, reanalysis is not required but the laboratory shall qualify the results of the affected samples.
When reporting results to the LOD, the concentration of each non-spiked target element in an interference check standard exceeds 10/3 their corresponding LOD for ICP analysis.
NR 149.47 Note
The examples for qualifying data listed in this section are common situations. Other situations may exist that could require qualification of data.
NR 149.47 History
History: CR 17-046: cr. Register February 2021 No. 782, eff. 6-29-21; correction in (2) (a) made under s. 35.17, Stats., Register February 2021 No. 782. NR 149.48
Quality control requirements for chemical testing. NR 149.48(1)(a)(a)
A laboratory shall establish a quality control program that includes the analysis of appropriate quality control samples and quality control procedures that define their practices. These quality control procedures shall be used to assess all the following:
The level of background contamination associated with the preparation and analysis of all samples.
The bias contributed to sample results by all preparation and analysis steps.
A laboratory may not adjust or correct the sample results by the recoveries of associated quality control samples or surrogates unless otherwise allowed by method, regulation, or covered program. A laboratory may not subtract analyte concentrations found in method blanks from sample results unless otherwise allowed by method, regulation, or covered program.
A laboratory shall document deviations from the laboratory's quality system or exceedances of quality control samples. To the extent the department's data systems allow, the deviations shall be communicated with the results.
A laboratory shall establish procedures for identifying and documenting preparation batches that facilitate determining compliance with the frequencies of quality control samples required under this chapter.
A laboratory shall determine the LOD for all tests performed except for any of the following:
Biochemical oxygen demand and carbonaceous biochemical oxygen demand.
Tests for which analyzing a fortified sample is impossible or impractical.