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9.6 Sample quality control for preparation and analysis The laboratory must also have procedures for documenting the effect of the matrix on method performance (precision, accuracy, method sensitivity). At a minimum, this should include the analysis of QC samples including a method blank, a matrix spike, a duplicate, and a laboratory control sample (LCS) in each analytical batch and the addition of surrogates to each field sample and QC sample when surrogates are used. Any method blanks, matrix spike samples, and replicate samples should be subjected to the same analytical procedures (Sec. 11.0) as those used on actual samples. 9.6.1 Documenting the effect of the matrix should include the analysis of at least one matrix spike and one duplicate unspiked sample or one matrix spike/matrix spike duplicate pair. The decision on whether to prepare and analyze duplicate samples or a matrix spike/matrix spike duplicate must be based on a knowledge of the samples in the sample batch. If samples are expected to contain target analytes, then laboratories may use one matrix spike and a duplicate analysis of an unspiked field sample. If samples are not expected to contain target analytes, laboratories should use a matrix spike and matrix spike duplicate pair. Consult Method 8000 for information on developing acceptance criteria for the MS/MSD. 9.6.2 A laboratory control sample (LCS) should be included with each analytical batch. The LCS consists of an aliquot of a clean (control) matrix similar to the sample matrix and of the same weight or volume. The LCS is spiked with the same analytes at the same concentrations as the matrix spike, when appropriate. When the results of the matrix spike analysis indicate a potential problem due to the sample matrix itself, the LCS results are used to verify that the laboratory can perform the analysis in a clean matrix. Consult Method 8000 for information on developing acceptance criteria for the LCS. 9.6.3 Also see Method 8000 for details on carrying out sample quality control procedures for preparation and analysis. In-house method performance criteria for evaluating method performance should be developed using the guidance found in Method 8000. |
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