RCRA Method 8280 for the analysis of chlorinated dibenzo-p-dioxins and dibenzofurans, as published in the Federal Register in April 1983, revealed the need for several modifications to allow for the determination of the target analytes in complex matrices, such as industrial sludge and still-bottom samples. Details of these modifications and of the subsequent application of the revised method to a limited number of samples which were analyzed in the course of a multilaboratory evaluation are reported. Further evaluation of RCRA Method 8280 for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans has been performed. The Method has been modified to provide for the quantitation of total tetra- through octa-chlorinated dioxins and dibenzofurans and has been applied to sample matrices derived from industrial polychlorophenol sources as well as to fly-ash, still-bottom, and Missouri soil samples. As an additional test of Method performance, an interlaboratory validation study was conducted in two parts. A two-part study was used because the Method had been extensively revised since its publication in the Federal Register, and it was felt that participating laboratories would be unfamiliar with some of the proposed procedures. The first phase was intended to allow the participants to acquire familiarization with the Method by analyzing relatively simple matrices for a few specified analytes which had been spiked into the samples. The second phase required the total quantitation of tetra- through octa-CDDs and CDFs in complex samples containing the analytes at both low (ppt) and extremely high (ppm) levels; no spiking was used for these samples. A method detection limit study using all available 13C12-labeled PCDD and PCDF isomers spiked into seven different sample matrices was also performed, and the results indicated both matrix and homolog specific differences. The revised Method 8280 has undergone a period of continual development; new documentation which will be reported includes Method performance data on complex samples from polychlorophenol use processes, results from an interlaboratory study of the revised method, and method detection limits of selected PCDDs and PCDFs in a variety of environmental and hazardous waste matrices.
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