United States Environmental Protection Agency Environmental Monitoring Systems Laboratory Las Vegas NV 89114 Research and Development EPA-600/S'4-84-038 June 1984 Project Summary Characterization of Hazardous Waste Sites—A Methods Manual: Volume III. Available Laboratory Analytical Methods Russell H. Plumb, Jr. A manual of available analytical pro- cedures was prepared as Volume 3 of the report. Characterization of Hazard- ous Waste Sites—A Methods Manual. This volume provides bench-level guid- ance for the preparation of hazardous waste, water, soil/sediment, biological tissue, and air samples, and suitable methods that can be used to analyze the resultant digests/extracts for 244 of the 359 substances listed in the Re- source Conservation and Recovery Act (RCRA) permit regulations. Each sam- ple preparation procedure and analytical method for the 929 analyte-matrix combinations that have been accumu- lated in this volume is classified as either evaluated or available based on the availability of precision and accuracy data. This Project Summary was developed by EPA's Environmental Monitoring Systems Laboratory, Las Vegas, NV. to announce key findings of the research project that is fully documented in a separate report of the same title fsee Project Report ordering information at back). Introduction The RCRA regulations concerned with the proper handling and disposal of hazardous wastes specify 359 chemical substances of concern. The bench-level guidance needed to implement the regula- tions should cover the topics of collection, preparation, and analysis of samples from diverse and complex matrices such as wastes, water, soil/sediment, biota, and air. However, existing analytical manuals are frequently dedicated to a single sample matrix (usually water) and nor- mally provide detailed guidance on the use of analytical procedures for only 50 to 125 substances. This manual is an expan- sion of these earlier efforts and provides guidance on the preservation and prepa- ration for more sample matrices, as well as analytical methods for more analytes. This project is part of a larger effort to prepare guidance manuals summarizing available information on hazardous waste site characterization, including prelimi- nary site assessment, sample collection, and sample analysis. Organization of the Manual Volume 3 of Characterization of Hazard- ous Waste Sites—A Methods Manual contains analytical procedures that are available for chemical characterization of samples obtained in hazardous waste site investigations. The text of this volume is divided into three chapters. Chapter 1 provides background information on the development of this manual and a dis- cussion of the format used to present each analytical procedure. Chapter 2 is divided into two main parts: the first provides guidance for handling and frac- tionation of hazardous waste samples in the laboratory and the second provides a protocol for general sample characteriza- tion, identifying potentially unsafe condi- tions that may be encountered when certain samples are analyzed (i.e., pres- ------- ence of strong oxidants, evolution of potentially toxic gases, and/or extreme pH values). Chapter 3 presents analytical procedures for specific analytes. A search of the literature, including both existing manuals and professional journals, was instituted to identify avail- able methods. The search focused on methods for the analysis of hazardous waste, water, soil/sediment, biological tissue, and air samples for any of the 359 compounds listed in the RCRA regula- tions. A procedure was considered suit- able for inclusion if the following criteria were met: • A demonstrated need exists for the procedure. • Detailed sample preparation guidance is provided for a specific sample matrix. • The analytical procedure is adequately described. • Precision and accuracy information is available to define the expected per- formance of the procedure. The first criterion was satisfied if the analyte was listed in Appendix VIII of the RCRA regulations.* The second criterion was considered to have been met if detailed sample preparation guidance (including digestion and/or extraction, and sample extract cleanup) was avail- able. The third requirement was satisfied if sufficient information on instrument operation (warm-up time, instrument calibration, and operating conditions) was located. The last criterion was satisfied if method performance data were available from one or more laboratories. The search produced 929 analyte- matrix combinations that fulfilled the criteria (163 analytes in waste, 244 analytes in water, 203 analytes in soil/ sediment, 217 analytes in biological tissue, and 102 analytes in air). These methods are presented in 24 analytical sections that are grouped as follows: Section 1-9: Organic Analytical Pro- cedures Section 10-18: Inorganic Analytical Pro- cedures Section 19-24: Sample Screening and Characterization Proce- dures The organic sections provide detailed procedures for the determination of vola- tile organic compounds, acid-extractable compounds, base/neutral compounds, pesticides and PCBs, organophosphorus pesticides, organonitrogen pesticides, phenyl acetic acids, dioxin, and poly- nuclear aromatic hydrocarbons. The in- organic sections provide detailed proce- dures for elemental determination by atomic absorption and inductively coupled plasma emission spectroscopy, and pro- cedures for mercury, methyl mercury, arsenic, selenium, cyanide, sulfide, and ammonia. Analytical methods in the screening section provide guidance for the determination of oxidant capacity, reductant capacity, acidity, alkalinity, conductivity, and percent moisture con- tent. A standard format was developed for presenting the information on sample preparation and the use of each analytical procedure. This approach permits analyt- ical research needs to be identified in several ways. Each method is classified as evaluated or available based on the amount of precision and accuracy data that was located. Methods classified as available are usable, but a need exists for a more extensive performance evaluation of the procedure. Research needs are further identified by reserving sections whenever sample preparation guidance could not be located for a particular analyte-matrix combination. Sections identified in this manner indicate a need for either a more extensive literature search, a performance evaluation of an existing procedure, or a methods develop- ment and evaluation effort. Finally, in- formation on sample preservation and preparation is presented in a flowchart associated with each analytical section. Gaps in these flowcharts identify needs for specific performance evaluations. This volume will require periodic up- dating as additional analytical procedures are located, as new methods are devel- oped and evaluated, and as additional performance data become available to update the classification of methods already included. •U.S. Environmental Protection Agency. "Hazardous Waste and Consolidated Permit Regulations," Federal Register. 40 CFR Part 261. May 19. 1980. pp. 33084-33133. ------- Russell H. Plumb, Jr., is with Lockheed Engineering and Management Services Company, Las Vegas, NV 89114. Werner F. Beckert is the EPA Project Officer (see below). The complete report, entitled "Characterization of Hazardous Waste Sites, A Methods Manual: Volume III. Available Laboratory Analytical Methods, "(Order No. PB 84-191 048; Cost: $47.00, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Environmental Monitoring Systems Laboratory U.S. Environmental Protection Agency P.O. Box 15027 Las Vegas, NV 89114 it U S GOVERNMENT PRINTING OFFICE, 1984 — 759-015/7722 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Official Business Penalty for Private Use $300 A«iŁNCY HtblUN 5 L >30 b DtAHBUKiM CHICAGO IL 1 ------- |