2012-227 - Laserfiche WebLink

Home Browse Search

7 . Instrument Calibration — In addition to calibration procedures specified in the analytical methods listed in the planning document, the GRANTEE shall ensure that the following requirements are met. a. All sample results shall be chronologically bracketed between acceptable calibration verifications. b. Initial Calibration Requirements (i) The minimum number of calibration standards required to calibrate each instrument used for the contracted analyses shall conform to the analytical method approved in the planning document. If the minimum number of calibration standards is not specified in the method, the number must be specified in the planning document and shall be consistent with the NELAC Chapter 5 standards. ( ii) Unless otherwise specified by the method, all sample results shall be based on the initial calibration curve responses. ( iii) If linear regressions are used, the correlation coefficient shall be equal to or greater than 0 .995 for all regressions . ( iv) Immediately after performing an initial calibration, the accuracy of the calibration shall be verified using a second source. A second source may be a standard, a Standard Reference Material (SRM), or other sample type with a verified concentration such as a QC Check Sample . Standards must have been prepared from a different lot or vendor. (v) The acceptance criteria for second-source verifications shall be specified in the planning document. (vi) Sample analysis cannot proceed if an initial calibration is unacceptable. c . Continuing Calibration Requirements : (i) When an initial calibration is not performed on the day of analysis, a continuing calibration standard shall be analyzed, evaluated and determined to be acceptable prior to analyzing samples . (ii) A continuing calibration standard shall be analyzed and evaluated at the end of the analytical run. (iii) The acceptance criteria for continuing calibration verifications shall be specified in the planning document. ( iv) For each analytical run, the analytical sensitivity must be evaluated using a continuing calibration standard prepared at the Contract-specified PQL. The analyzed value of this standard must be within 70% — 130% of the expected value. If this PQL check fails, the blank and associated sample results must be reported as "estimated" per Chapter 62460, F. A.C . unless the affected results are at least 10 times the absolute value of the observed bias of the PQL check. (v) If a continuing calibration verification fails, samples not chronologically bracketed by acceptable calibration verifications must be reanalyzed or appropriately qualified. d. Sample results below the Contract-specified PQL and above the highest calibration standard shall be appropriately qualified. 8 . Quality Control Blanks a. If a Contracted analyte is detected in any analytical QC blank, the sample results that are associated with the blank must be reported with the appropriate qualifier from Chapter 62460, F .A.C . , unless the affected sample concentrations are at least 10 times higher than the calculated QC blank concentration. b. Sample results must be chronologically bracketed with acceptable beginning and ending analytical QC blanks . c. If a Contracted analyte is detected in the field blank, equipment blank or trip blank, the result must be confirmed by reanalyzing a new aliquot of the blank unless the sample concentration results associated with the blank are at least 10 times the calculated blank concentration. The laboratory must investigate the blank contamination to determine that positive blank results are not due to a laboratory error and report the affected samples and field-generated blank results with appropriate qualifiers and/or comments. 9. If any quality control measure or calibration verification fails (including those specified above), samples that are associated with the failure must be reanalyzed, if possible. Sample data that are associated with a failed quality control measure or calibration must be appropriately qualified as specified in Chapter 62460, F.A . C . An explanatory comment must be attached to the final report for each result that has a qualifier code other than U, I, or A . Any additional qualifier codes used but not explicitly listed in Chapter 62460, F .A .C . must be identified and defined in the report. 10 . The reported MDL and PQL for each sample must be adjusted for dilution factors and any relevant preparation weights and volumes . 11 . Field QC duplicates or replicates - The GRANTEE shall ensure that field duplicates (not to be confused with laboratory duplicates) are analyzed. All field duplicate results greater than the contracted PQL should agree within 20% RPD for each measured analyte . In the event that field duplicate agreement is not observed, the Revision Date: 02/09 DEP Agreement No. G0353, Attachment J. Page 7 of 14