Mine Health and Safety Act, 1996 (Act No. 29 of 1996)

Certain quality control checks should be performed with each sample set to further support the reported results on actual field samples. The exact number and nature of these checks depend on the specific method and circumstances under consideration and, should be thought of as an integral part of the method itself (i.e. a measurement should not be considered completed without the quality control checks also being completed). Each analyst must take an independent responsibility for assuring that the analytical quality control system works. This can be accomplished by using known spiked samples that closely simulate field samples with regard to concentration and interferences. Since the analyst is most familiar with the methods being used and should know what range of recoveries to expect, problems with the system can be detected early. The following additional quality control checks should be considered as appropriate:

First, and perhaps most important in the area of quality control, a laboratory must have adequate measurement procedures. These methods should be written so that there is no doubt in the analyst's mind of the exact steps which must be performed and so that future references to the work can be as exact as possible. The methods used should be evaluated, where possible (either by the laboratory itself or by some other organisation), to verify that the methods perform satisfactorily. Factors that could be evaluated include the recovery of the analyte of interest from both spiked samples and generated samples, the stability of collected samples or possible interferences for accurate use of the method. Methods should be tested for ruggedness so that critical steps in the analysis can be identified. Experimental designs have been published which permit rapid evaluation of a number of factors involved in the analysis.

Standard solutions may be for either identification or quantitation of the analyte of interest. The bulk material used for preparation of standards should be of sufficient purity to avoid errors in the identification or quantitation. Where available, Standard Reference Materials or other well-characterized standards are useful for assuring that results are consistent with other organisations and agencies. Laboratory reagents and standards should also be properly labelled with contents, and receipt and expiration dates.

For quantitation, sufficient numbers of standards should be prepared so that adequate confidence intervals on reported values can be obtained. As a guideline, it is recommended that calibration curves be prepared with triplicate points at each of at least five different concentration levels. The standard curve should be prepared so that linearity can be assured over the range of the curve. Also, it is important that the concentration of standard solutions be chosen to bracket the actual samples. In this way, extrapolation outside the range of standards is avoided. The concentration of standard solutions should be chosen to be consistent with the purpose of the sampling. That is, if it is desired to demonstrate whether exposure standards are being met, then the standard curve should be constructed to bracket the concentrations which would be encountered at or near the applicable exposure standard. If it is desired to demonstrate whether a compound is present in the atmosphere being sampled, then the calibration curve should be constructed closer to the limit of detection. During measurement, working standards should be interspersed with field samples. In this way, it should be possible to detect if instrument drift becomes significant. Internal standards are useful for correcting instrument response for the actual amount of sample injected into a chromatograph. The internal standard should be chosen so that its retention time is reasonably close, without peak overlap, to the peak of interest.

A particular analysis may involve several types of "blank" measurements including reagent blanks, media blanks or field blanks. Reagent blanks measure the signal contribution from solvents, acids or other reagents used by the laboratory in preparing samples for analysis. Media blanks measure the signal contribution from the collection media (impinger solution, filter, sorbent tube, etc.) and field blanks measure signal contribution of the media plus any contamination that may have occurred during handling, shipping and storage before analysis. The nature and number of blank measurements will depend on the method and circumstances, but the purpose of all blank measurements is to help prevent errors in identification and quantitation of field samples.

Blind samples are prepared by someone other than the analyst performing the measurement and are to provide an independent check on the accuracy and precision of the measurement.

If blind samples cannot be prepared with confidence, their use should be avoided. in these cases, confusion may result when discrepancies occur and it will not be possible to say for certain whether the measurement or the blind sample was in error.

The results should be used in conjunction with control charting techniques to identify errors or malfunctions in the system. To accomplish this goal, quality assurance personnel should work closely with laboratory personnel to quickly identify and eliminate trouble spots.

It will not always be possible to isolate the source of error in the results of a blind sample. In these instances, it should be recognized that it will not be possible to defend quantitative results for that particular sample set; therefore, reporting of results where these discrepancies occur should be avoided.

Recovery studies should be performed as a part of the measurement whenever the analyte of interest must be liberated or separated from the sampling media. The analyte of interest should be added to the media at levels consistent with the field samples. These "spiked" samples should then be treated in the same manner as the field samples. Corrections for recovery should be made whenever the measured recovery is significantly different from 100%. Even if recovery has historically been 100%, recovery studies can be useful as additional analytical and calculation checks. It is often helpful for a laboratory to maintain a record of past recovery studies so that current data may be compared for discrepancies. Samples for which estimated recovery is less than 75% should be reported as "semi quantitative".

Duplicate preparations of bulk materials are useful as an indication of the uniformity of the bulk material. Duplicate injections or measurements from air samples are of lesser importance since preparations from air samples are generally fairly uniform hi nature. True duplicates of air samples are useful as an indication of the uniformity of the atmosphere being sampled.