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JUN 2 3 1997 Bureau of Reclamation Reclamation Service Center Preparing Soil Samples for Volatile Organic Compound Analysis Alan D, Hewitt April 1997 $ Abstract: Three equilibrium headspace and three sol­vent extraction methods of preparing soil samples for determining volatile organic compounds (VOCs) were compared. Soil samples were spiked with five gasoline range aromatic compounds and four chlorinated com­pounds using Iwo different laboratory procedures that limit volatilization and biodegradation losses. All com­parisons were made with sample triplicates of one or more soil types. Recovery efficiencies for the prepara-tion methods depended on soil organic carbon content, octanol-water partition coefficients of specific analytes, length of solvent extraction, and the spiking procedure used. In general, methanol extraction was the most robust method for recovering spiked VOCs. Recovery efficiencies for VOCs with tetraethylene glycol dimethyl ether and poly(propylene)glycol, as well as three equi­librium headspace methods, varied with the parameters tested. How to get copies of CRREL technical publications: Department of Defense personnel and contractors may order reports through the Defense Technical Information Center: DTIC-BR SUITE 0944 8725 JOHN J KINGMAN RD FT BELVOIRVA 22060-6218 Telephone 1 800 225 3842 E-mail help@dtic.mil msorders@dtic.mil WWW http://www.dtic.dla.mil/ All others may order reports through the National Technical Information Service: NTIS 5285 PORT ROYAL RD SPRINGFIELD VA 22161 Telephone 1 703 487 4650 1 703 487 4639 (TDD for the hearing-impaired) E-mail orders@ntis.fedworld.gov WWW http://www.fedworld.gov/ntis/ntishome.html A complete list of all CRREL technical publications is available from: USACRREL (CECRL-LP) 72 LYME RD HANOVER NH 03755-1290 Telephone 1 603 646 4338 E-mail techpubs@crrel.usace.army.mil For information on all aspects of the Cold Regions Research and Engineering Laboratory, visit our World Wide Web site: http://www.crrel.

JUN - 3 1997 Bureau of Reclamation Reclamation Service Center Detecting Metallic Primary Explosives with a Portable X-ray Fluorescence Spectrometer Alan D. Hewitt April 1997 Abstract: X-ray fluorescence spectrometry (XRF) analysis is a practical means of performing in-situ screening to establish the presence of high concentra­tions (>0.1% or 1000 ppm) of lead (Pb) and/or mer­cury (Hg). These two metals are of special military interest because they are constituents in three primary explosives: lead azide [Pb(N3) 2], lead styphnate (CeHOeNsPb), and mercury fulminate [Hg(CNO>2] • The success of in-situ XRF analysis to perform this task depends on instrumental sensitivity, selectivity, effec­tive sample volume, transportability, and user friend-liness. Laboratory experiments established that the MAP-3 XRF spectrum analyzer (SCITEC Corporation) is well-suited for this application. This instrument is self-contained, portable, and equipped with a Co-57 source that allows for a simultaneous analysis of both the K and L energy lines of Pb and Fig, among other metals. Laboratory experiments established that high concentrations of Pb and Hg could be detected in an active sample area of cylindrical shape, approximately 1.0 cm In diameter and 1.5 cm In depth. How to get copies of CRREL technical publications: Department of Defense personnel and contractors may order reports through the Defense Technical Information Center: DTIC-BR SUITE 0944 8725 JOHN J KINGMAN RD FT BELVOIRVA 22060-6218 Telephone 1 800 225 3842 E-mail help@dtic.mil msorders@dtlc.mil WWW http://www.dtlc.dla.mil/ All others may order reports through the National Technical Information Service: NTIS 5285 PORT ROYAL RD SPRINGFIELD VA 22161 Telephone 1 703 487 4650 1 703 487 4639 (TDD for the hearing-impaired) E-mail orders@ntls.fedworld.gov WWW http ://www.fedworld .gov/ntls/ntlshome. html A complete list of all CRREL technical publications is available from: USACRREL (CECRL-LP) 72 LYME RD HANOVER NH 03755-1290 Tele

Ti GB 2401 .C6s No.97-12 1997 Estimating the Total Concentration of Volatile Organic Compounds in Soil A Decision Tool for Sample Handling Alan D. Hewitt and Nicole J.E. Lukash April 1997 Abstract: This report describes an on-site method of estimating the total concentration of Volatile Organic Compounds (VOCs) in soil, relative to a site-specific 0.2-mg/kg standard. This decision tool allows on-site sampling activities to incorporate the appropriate soil sample collection and handling protocols required by different methods of instrumental analysis. Coupling a rapid method for estimating the total VOC concentra­tion with sampling procedures that limit substrate dis­aggregation and exposure complements efforts to achieve site-representative estimates for vadose zone contamination. How to get copies of CRREL technical publications: Department of Defense personnel and contractors may order reports through the Defense Technical Information Center: DTIC-BR SUITE 0944 8725 JOHN J KINGMAN RD FT BELVOIRVA 22060-6218 Telephone 1 800 225 3842 E-mail help@dtic.mil msorders@dtic.mil WWW http://www.dtic.dla.mil/ All others may order reports through the National Technical Information Service: NTIS 5285 PORT ROYAL RD SPRINGFIELD VA 22161 Telephone 1 703 487 4650 1 703 487 4639 (TDD for the hearing-impaired) E-mail orders@ntis.fedworld.gov WWW http://www.fedworld.gov/ntis/ntishome.html A complete list of all CRREL technical publications is available from: USACRREL (CECRL-LP) 72 LYME RD HANOVER NH 03755-1290 Telephone 1 603 646 4338 E-mail techpubs@crrel.usace.army.mil For information on all aspects of the Cold Regions Research and Engineering Laboratory, visit our World Wide Web site: http://www.crrel.usace.army.mil ¿'^'Special Report 97-12 \cffi BUREAU OF RECLAMATION DENVER LIBRARY US Army Corps of Engineers® Cold Regions Research & Engineering Laboratory Estimating the Total Concentration of Volatile Organic Compounds in Soil A Decision Tool for Sample Handling Alan D. Hewitt an

1994 Screening for Metals by X-Ray Fluorescence Spectrometry Using a Single Calibration Standard Alan D. Hewitt July 1994 Abstract Analysis for copper, zinc, arsenic and lead was performed on a variety of solid particle matrices using a portable, high-resolution X-ray fluorescence (XRF) spectrometer. All quantitative determinations were based on an instrumental calibration method that uses a single certified reference material to establish elemental response factors and the Compton Ka peak to normalize for matrix discrepancies. This simple approach to XRF analysis circumvents the need to acquire matrix-matched standardsfor either empirical coefficients orfundamen-tal parameter methods of calibration. Preliminary results show that response factor/Compton Ka peak normalization is a promising approach when screen­ing for these metals in soils, dust, paint chips and incinerated sludge. DATE DUE GAYLORD PRINTED IN U.S.A. For conversion of SI metric units to U.S./British customary units of measurement consult ASTM Standard E380-89a, Standard Practice for Use of the International System o f Units, published by the American Society for Testing and Materials, 1916 Race St., Philadelphia, Pa. 19103. ,¿3 sOo.W'^o iw Y