15.2: Quality Control

Quality control encompasses all activities that bring an analysis into statistical control. The most important facet of quality control is a set of written directives that describe relevant laboratory-specific, technique-specific, sample-specific, method-specific, and protocol-specific operations. Good laboratory practices (GLPs) describe the general laboratory operations that we must follow in any analysis. These practices include properly recording data and maintaining records, using chain-of-custody forms for samples, specifying and purifying chemical reagents, preparing commonly used reagents, cleaning and calibrating glassware, training laboratory personnel, and maintaining the laboratory facilities and general laboratory equipment.

For one example of quality control, see Keith, L. H.; Crummett, W.; Deegan, J., Jr.; Libby, R. A.; Taylor, J. K.; Wentler, G. “Principles of Environmental Analysis,” Anal. Chem. 1983, 55, 2210–2218. This article describes guidelines developed by the Subcommittee on Environmental Analytical Chemistry, a subcommittee of the American Chemical Society’s Committee on Environmental Improvement.

Good measurement practices (GMPs) describe those operations specific to a technique. In general, GMPs provide instructions for maintaining, calibrating, and using equipment and instrumentation. For example, a GMP for a titration describes how to calibrate the buret (if required), how to fill the buret with titrant, the correct way to read the volume of titrant in the buret, and the correct way to dispense the titrant.

The directions for analyzing a specific analyte in a specific matrix are described by a standard operations procedure (SOP). The SOP indicates how we process the sample in the laboratory, how we separate the analyte from potential interferents, how we standardize the method, how we measure the analytical signal, how we transform the data into the desired result, and how we use quality assessment tools to maintain quality control. If the laboratory is responsible for sampling, then the SOP also states how we must collect, process, and preserve the sample in the field. An SOP may be developed and used by a single laboratory, or it may be a standard procedure approved by an organization such as the American Society for Testing Materials or the Federal Food and Drug Administration. A typical SOP is provided in the following example.

Example 15.2.1

Provide an SOP for the determination of cadmium in lake sediments using atomic absorption spectroscopy and a normal calibration curve.

Solution

Collect sediment samples using a bottom grab sampler and store them at 4^oC in acid-washed polyethylene bottles during transportation to the laboratory. Dry the samples to constant weight at 105^oC and grind them to a uniform particle size. Extract the cadmium in a 1-g sample of sediment by adding the sediment and 25 mL of 0.5 M HCl to an acid-washed 100-mL polyethylene bottle and shaking for 24 h. After filtering, analyze the sample by atomic absorption spectroscopy using an air–acetylene flame, a wavelength of 228.8 nm, and a slit width of 0.5 nm. Prepare a normal calibration curve using five standards with nominal concentrations of 0.20, 0.50, 1.00, 2.00, and 3.00 ppm. Periodically check the accuracy of the calibration curve by analyzing the 1.00-ppm standard. An accuracy of \(\pm\) 10% is considered acceptable.

Although an SOP provides a written procedure, it is not necessary to follow the procedure exactly as long as we are careful to identify any modifications. On the other hand, we must follow all instructions in a protocol for a specific purpose (PSP)—the most detailed of the written quality control directives—before an agency or a client will accept our results. In many cases the required elements of a PSP are established by the agency that sponsors the analysis. For example, a lab working under contract with the Environmental Protection Agency must develop a PSP that addresses such items as sampling and sample custody, frequency of calibration, schedules for the preventive maintenance of equipment and instrumentation, and management of the quality assurance program.

Two additional aspects of a quality control program deserve mention. The first is that the individuals responsible for collecting and analyzing the samples can critically examine and reject individual samples, measurements, and results. For example, when analyzing sediments for cadmium (see the SOP in Example 15.2.1 ) we might choose to screen sediment samples, discarding a sample that contains foreign objects—such as rocks, twigs, or trash—replacing it with an additional sample. If we observe a sudden change in the performance of the atomic absorption spectrometer, we may choose to reanalyze the affected samples. We may also decide to reanalyze a sample if the result of its analysis clearly is unreasonable. By identifying those samples, measurements, and results subject to gross systematic errors, inspection helps control the quality of an analysis.

The second additional consideration is the certification of an analyst’s competence to perform the analysis for which he or she is responsible. Before an analyst is allowed to perform a new analytical method, he or she may be required to analyze successfully an independent check sample with acceptable accuracy and precision. The check sample is similar in composition to samples that the analyst will analyze later, with a concentration that is 5 to 50 times that of the method’s detection limit.