Illustrated here is an example of a prescriptive approach to quality assurance for laboratories monitoring waters and wastewaters, adapted from Environmental Monitoring and Support Laboratory, U. S. Environmental Protection Agency, “Handbook for Analytical Quality Control in Water and Wastewater Laboratories,” March 1979.
Two samples, A and B, are collected at the sample site. Sample A is split into two equal-volume samples, A1 and A2. Sample B is also split into two equal-volume samples, one of which, BSF, is spiked in the field with a known amount of analyte. A field blank, DF, also is spiked with the same amount of analyte. All five samples (A1, A2, B, BSF, and DF) are preserved if necessary and transported to the laboratory for analysis.
After returning to the lab, the first sample that is analyzed is the field blank. If its spike recovery is unacceptable—an indication of a systematic error in the field or in the lab—then a laboratory method blank, DL, is prepared and analyzed. If the spike recovery for the method blank is unsatisfactory, then the systematic error originated in the laboratory; this is something we can find and correct before proceeding with the analysis. An acceptable spike recovery for the method blank, however, indicates that the systematic error occurred in the field or during transport to the laboratory, casting uncertainty on the quality of the samples. The only recourse is to discard the samples and return to the field to collect new samples.
If the field blank is satisfactory, then sample B is analyzed. If the result for B is above the method’s detection limit, or if it is within the range of 0.1 to 10 times the amount of analyte spiked into BSF, then a spike recovery for BSF is determined. An unacceptable spike recovery for BSF indicates the presence of a systematic error involving the sample. To determine the source of the systematic error, a laboratory spike, BSL, is prepared using sample B, and analyzed. If the spike recovery for BSL is acceptable, then the systematic error requires a long time to have a noticeable effect on the spike recovery. One possible explanation is that the analyte has not been properly preserved or it has been held beyond the acceptable holding time. An unacceptable spike recovery for BSL suggests an immediate systematic error, such as that due to the influence of the sample’s matrix. In either case the systematic errors are fatal and must be corrected before the sample is reanalyzed.
If the spike recovery for BSF is acceptable, or if the result for sample B is below the method’s detection limit, or outside the range of 0.1 to 10 times the amount of analyte spiked in BSF, then the duplicate samples A1 and A2 are analyzed. The results for A1 and A2 are discarded if the difference between their values is excessive. If the difference between the results for A1 and A2 is within the accepted limits, then the results for samples A1 and B are compared. Because samples collected from the same sampling site at the same time should be identical in composition, the results are discarded if the difference between their values is unsatisfactory, and accepted if the difference is satisfactory.
In total, this protocol requires four to five evaluations of quality assessment data before the result for a single sample is accepted, a process we must repeat for each analyte and for each sample. Clearly this is a lengthy and time-consuming process.
About Author
