A microwave-assisted method for preparing samples for determination of elements In solid waste has been developed (draft EPA Method 3051). Validation of the sample preparation method was performed through a collaborative study to determine its precision and accuracy. Fifteen independent laboratories digested 4 National Institute of Standards and Technology (NIST) standard reference materials (SRMs) and 1 solvent recovery waste in duplicate. Digestates were analyzed for 19 elements using inductively coupled plasma (ICP) emission spectroscopy. The precision and bias of the method were evaluated. When compared with an open vessel hot-plate digestion method (SW-846 Method 3050), the microwave method produced similar analytical results with better overall precision. Bias for the 1 sample that allowed this determination was found to be excellent.
The techniques which are typically used to prepare RCRA wastes for analysis for metals and other elements are generally relatively time consuming, requiring several hours to several days to complete. They also often involve the use of acid digestions and thermal decomposition steps which may result in analyte losses, incomplete recoveries, or sample contamination. These limitations are well known to the analytical community and to the end users of these data in EPA, States, and industry. The resulting inefficiency of these techniques reduces laboratory sample throughput, drives up the cost of analytical testing, and impedes decision making. Given these concerns, the OSW Methods Section is interested in developing cost effective sample preparation techniques for metals and other elements in environmental and process waste samples. Once developed, these techniques can then be written as methods for inclusion in Test Methods for Evaluation of Solid Waste SW-846 and made available to the user community. This paper reports on the evaluation of a microwave assisted sample preparation method for determining elements in solid waste. The Method was evaluated for microwave digestion of sediments, sludges, soils, and oils.
The techniques that are typically used to prepare RCRA wastes for analysis for metals and other elements are generally relatively time consuming, requiring several hours to several days to complete. They also often involve the use of acid digestions and thermal decomposition steps which may result in analyte losses, incomplete recoveries, or sample contamination. These limitations are well known to the analytical community and to the end users of these data in the U.S. EPA, States, and industry. The resulting inefficiency of these techniques reduces laboratory sample throughput, drives up the cost of analytical testing and impedes decisionmaking. Given these concerns, the OSW Methods Section is interested in developing cost-effective sample preparation techniques for metals and other elements in environmental and process waste samples. Once developed, these techniques can then be written as methods for inclusion in the U.S. EPA “Test Methods for Evaluation of Solid Waste” (SW-846) [1] and made available to the user community.
A microwave-assisted sample preparation method for determining elements in solid waste has been developed (Method 3051). This paper reports on the validation of this method by a collaborative study to determine its precision and accuracy. Both qualitative and quantitative aspects of the method were assessed. Qualitative factors evaluated were ease of use and time requirements. Quantitative factors evaluated were the bias and the precision (single laboratory and total). The method was compared with U.S. EPA Method 3050, an open-vessel, hot plate digestion method.
A quality assurance program was developed for two grantee laboratories studying the herbicides atrazine and linuron in Chesapeake Bay water. Proposed methodologies were evaluated by performance and system audits. The objectives of the quality assurance program and the results of the audit program are discussed.
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