You are here:
CAPILLARY GAS CHROMATOGRAPHY-ATOMIC EMISSION DETECTION METHOD FOR THE DETERMINATION OF PENTYLATED ORGANOTIN COMPOUNDS: INTERLABORATORY STUDY
Citation:
Liu, Y., V. Lopez-Avila, M. Alcaraz, AND W. Beckert. CAPILLARY GAS CHROMATOGRAPHY-ATOMIC EMISSION DETECTION METHOD FOR THE DETERMINATION OF PENTYLATED ORGANOTIN COMPOUNDS: INTERLABORATORY STUDY. Journal of the Association of Official Analytical Chemists International 78(5):1275-1285, (1995).
Description:
A capillary gas chromatography-atomic emission detection (GC-AED) method was developed for the U. S. Environmental Protection Agency's Environmental Monitoring Systems Laboratory in Las Vegas, NV, for determination of selected organotin compounds. Here we report on an interlaboratory study to establish whether these compounds can reliably be detected and quantitated by this method and to establish the interlaboratory precision and accuracy with currently available instrumentation. A blind, balanced-replicate design was selected for this study, based on a recommendation of AOAC INTERNATIONAL. Ten laboratories volunteered for this study. Each laboratory received 5 calibration standards (pentylated organotin compounds), 3 pentylated soil or sediment extacts (prepared in our laboratory by an in situ complexation/supercritical fluid extraction method), and 1 pentylation blank. The participating laboratories analyzed the extracts according to our instructions and submitted the data to us for statistical analysis. Of 720 individual sample results, the number of outliers identified with the Cochran test was 60 (8.3%). Two laboratories accounted for most of the outliers. Results indicate that good chromatographic performance was achieved regardless of the type of injection inlet; however, electronic pressure control was needed to achieve acceptable chromatography for tetracyclohexyltin and tetraphenyltin. The intralaboratory precisions of the GC-AED method ranged from 1.3 to 22% relative standard deviation (RSD), depending on the compound. The interlaboratory method precisions ranged from 11 to 40% RSD over the concentraion range tested.