Interlaboratory and Intralaboratory Variability in the Analysis of Mercury in Coal.

Abstract

With the passage of the 1990 Clean Air Act Amendments (CAAA), accurate determination of the concentration of mercury in coal has become an increasingly important issue. To address this issue, CONSOL R&D conducted a round robin analytical program to determine the interlaboratory and intralaboratory variability in the measurement of mercury in coal. CONSOL supplied homogeneous splits of Pittsburgh and Illinois #6 seam coals, and the NIST 1632b coal standard to eleven laboratories, twice each, over a one-year period. A twelfth laboratory analyzed the coals once. A European coal standard, certified for mercury, was analyzed at the completion of the round robin study to evaluate accuracy. The round robin participants included representatives from industry, government, and academia. The laboratories, which are experienced in mercury-in-coal analysis, used various state-of-the-art sample preparation and analysis procedures in the study. The round robin results indicate that a substantial level of variability exists in the mercury-in-coal determination. Earlier studies1 found similar results. The relative intralaboratory repeatability was 0.02 ppm and the relative interlaboratory reproducibility ranged from 0.04 to 0.05 ppm. The study showed that laboratory variability can be greatly skewed by outlier values. Fifty-six percent of the results for the European coal standard fell within a 95% confidence interval of the standard (0.138 ± 0.11 ppm). These results indicate that accuracy is not method-dependent.