Section NR 149.446 - Continuing instrument calibration requirements(1) GENERAL PROVISIONS. 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: (a) 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.(b) 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.(c) Continuing calibration verification is not required for technologies when there are no initial calibrations established.(d) If an LCS also serves as a CCV standard, the acceptance criteria of the CCV standard shall be used.(2) FREQUENCY. (a) 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.(b) 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.(3) MINIMUM NUMBER OF STANDARDS AND CONCENTRATION LEVELS. (a) For linear and quadratic model calibration functions, the laboratory shall a Note: Linear calibration models include electrometric technologies (pH and ion selective electrode), average response factor, average calibration factor, linear regression, and least squares analysis.
nalyze at least a single CCV standard. The concentration of the standard shall be within the range established during the initial calibration.(b) 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.(4) VERIFYING ACCURACY. (a) 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.(b) 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.(5) ACCURACY CORRECTIVE ACTION. (a) When a CCV standard fails, the laboratory shall do any of the following: 1. Perform corrective action and reanalyze the CCV standard. If the CCV standard does not pass, an initial calibration shall be performed.2. 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.(6) EVALUATING SENSITIVITY. 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).Wis. Admin. Code Department of Natural Resources NR 149.446
Adopted by, CR 17-046: cr. Register February 2021 No. 782, eff. 6/29/2021