Assessment of Agent Monitoring Strategies for the
Blue Grass and Pueblo Chemical Agent Destruction
Pilot Plants

Committee on Assessment of Agent Monitoring Strategies for the Blue Grass and
Pueblo Chemical Agent Destruction Pilot Plants


Board on Army Science and Technology

Division on Engineering and Physical Sciences

NATIONAL RESEARCH COUNCIL
OF THE NATIONAL ACADEMIES

THE NATIONAL ACADEMIES PRESS
Washington, D.C.
www.nap.edu



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Assessment of Agent Monitoring Strategies for the Blue Grass and Pueblo Chemical Agent Destruction Pilot Plants Committee on Assessment of Agent Monitoring Strategies for the Blue Grass and Pueblo Chemical Agent Destruction Pilot Plants Board on Army Science and Technology Division on Engineering and Physical Sciences THE NATIONAL ACADEMIES PRESS Washington, D.C. www.nap.edu

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THE NATIONAL ACADEMIES PRESS 500 FIFTH STREET, NW Washington, DC 20001 NOTICE: The project that is the subject of this report was approved by the Governing Board of the National Research Council, whose members are drawn from the councils of the National Academy of Sciences, the National Academy of Engineering, and the Institute of Medicine. The members of the committee responsible for the report were chosen for their special competences and with regard for appropriate balance. This study was supported by Contract No. W911NF-11-C-0033 between the National Academy of Sciences and the U.S. Army. Any opinions, findings, conclusions, or recommendations expressed in this publication are those of the author(s) and do not necessarily reflect the views of the organizations or agencies that provided support for the project. International Standard Book Number-13: 978-0-309-25985-9 International Standard Book Number-10: 0-309-25985-1 Limited copies of this report are available from Board on Army Science and Technology, National Research Council, 500 fifth Street, NW, Room 940, Washington, DC 20001; (202) 334-3118. Additional copies of this report are available from the National Academies Press, 500 Fifth Street, NW, Keck 360, Washington, DC 20001; (800) 624-6242 or (202) 334-3313; http://www.nap.edu. Copyright 2012 by the National Academy of Sciences. All rights reserved. Printed in the United States of America

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The National Academy of Sciences is a private, nonprofit, self-perpetuating society of distinguished scholars engaged in scientific and engineering research, dedicated to the furtherance of science and technology and to their use for the general welfare. Upon the authority of the charter granted to it by the Congress in 1863, the Academy has a mandate that requires it to advise the federal government on scientific and technical matters. Dr. Ralph J. Cicerone is president of the National Academy of Sciences. The National Academy of Engineering was established in 1964, under the charter of the National Academy of Sciences, as a parallel organization of outstanding engineers. It is autonomous in its administration and in the selection of its members, sharing with the National Academy of Sciences the responsibility for advising the federal government. The National Academy of Engineering also sponsors engineering programs aimed at meeting national needs, encourages education and research, and recognizes the superior achievements of engineers. Dr. Charles M. Vest is president of the National Academy of Engineering. The Institute of Medicine was established in 1970 by the National Academy of Sciences to secure the services of eminent members of appropriate professions in the examination of policy matters pertaining to the health of the public. The Institute acts under the responsibility given to the National Academy of Sciences by its congressional charter to be an adviser to the federal government and, upon its own initiative, to identify issues of medical care, research, and education. Dr. Harvey V. Fineberg is president of the Institute of Medicine. The National Research Council was organized by the National Academy of Sciences in 1916 to associate the broad community of science and technology with the Academy's purposes of furthering knowledge and advising the federal government. Functioning in accordance with general policies determined by the Academy, the Council has become the principal operating agency of both the National Academy of Sciences and the National Academy of Engineering in providing services to the government, the public, and the scientific and engineering communities. The Council is administered jointly by both Academies and the Institute of Medicine. Dr. Ralph J. Cicerone and Dr. Charles M. Vest are chair and vice chair, respectively, of the National Research Council www.national-academies.org

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COMMITTEE ON ASSESSMENT OF AGENT MONITORING STRATEGIES FOR THE BLUE GRASS AND PUEBLO CHEMICAL AGENT DESTRUCTION PILOT PLANTS CHARLES E. KOLB, Chair, Aerodyne Research, Inc., Billerica, Massachusetts JESSE L. BEAUCHAMP (NAS), California Institute of Technology, Pasadena ROBERT A. BEAUDET, University of Southern California, Pasadena JOAN B. BERKOWITZ, Farkas Berkowitz and Company, Washington, D.C. HAO CHEN, Ohio University, Athens ADRIENNE T. COOPER, Florida Agricultural and Mechnical University, Tallahassee FACUNDO M. FERNANDEZ, Georgia Institute of Technology, Atlanta ROBERT D. GIBBONS (IOM), University of Chicago JOHN A. MCLEAN, Vanderbilt University, Nashville, Tennessee MAX D. MORRIS, Iowa State University, Ames DONALD W. MURPHY (NAE), Bell Laboratories, Lucent Technologies (retired), Davis, California C. SHANE REESE, Brigham Young University, Mapleton, Utah LORENZ R. RHOMBERG, Gradient, Cambridge, Massachusetts ALBERT A. VIGGIANO, Air Force Research Laboratory, Kirtland AFB, New Mexico Staff HARRISON T. PANNELLA, Study Director NIA D. JOHNSON, Senior Research Associate ANN F. LARROW, Research Assistant v

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BOARD ON ARMY SCIENCE AND TECHNOLOGY ALAN H. EPSTEIN, Chair, Pratt & Whitney, East Hartford, Connecticut DAVID M. MADDOX, Vice Chair, Independent Consultant, Arlington, Virginia DUANE ADAMS, Independent Consultant, Carnegie Mellon University (retired), Arlington, Virginia ILESANMI ADESIDA, University of Illinois at Urbana-Champaign MARY E. BOYCE, Massachusetts Institute of Technology, Cambridge EDWARD C. BRADY, Strategic Perspectives, Inc., Fort Lauderdale, Florida W. PETER CHERRY, Independent Consultant, Ann Arbor, Michigan EARL H. DOWELL, Duke University, Durham, North Carolina JULIA D. ERDLEY, Pennsylvania State University, State College LESTER A. FOSTER, Electronic Warfare Associates, Herndon, Virginia JAMES A. FREEBERSYSER, BBN Technology, St. Louis Park, Minnesota RONALD P. FUCHS, Independent Consultant, Seattle, Washington W. HARVEY GRAY, Independent Consultant, Oak Ridge, Tennessee JOHN J. HAMMOND, Lockheed Martin Corporation (retired), Fairfax, Virginia RANDALL W. HILL, JR., University of Southern California Institute for Creative Technologies, Playa Vista JOHN W. HUTCHINSON, Harvard University, Cambridge, Massachusetts MARY JANE IRWIN, Pennsylvania State University, University Park ROBIN L. KEESEE, Independent Consultant, Fairfax, Virginia ELLIOT D. KIEFF, Channing Laboratory, Harvard University, Boston, Massachusetts WILLIAM L. MELVIN, Georgia Tech Research Institute, Smyrna ROBIN MURPHY, Texas A&M University, College Station SCOTT PARAZYNSKI, University of Texas Medical Branch, Galveston RICHARD R. PAUL, Independent Consultant, Bellevue, Washington JEAN D. REED, Independent Consultant, Arlington, Virginia LEON E. SALOMON, Independent Consultant, Gulfport, Florida JONATHAN M. SMITH, University of Pennsylvania, Philadelphia MARK J.T. SMITH, Purdue University, West Lafayette, Indiana MICHAEL A. STROSCIO, University of Illinois, Chicago DAVID A. TIRRELL, California Institute of Technology, Pasadena JOSEPH YAKOVAC, President, JVM LLC, Hampton, Virginia Staff BRUCE A. BRAUN, Director CHRIS JONES, Financial Manager DEANNA P. SPARGER, Program Administrative Coordinator vi

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Preface More than 25 years ago, in 1986, the U.S. Army began destruction of its nearly 30,000-ton legacy of stockpiled chemical agents, stored in approximately 3 million individual munitions as well as numerous bulk agent containers. The nation's chemical weapons demilitarization effort has succeeded in destroying the chemical munitions and bulk agent stored at six of the eight chemical agent depots located in the continental United States. Chemical weapons that had been deployed abroad and relocated to a storage depot on Johnston Atoll, southwest of Hawaii, have also been successfully destroyed. To date, 90 percent of the original U.S. stockpile has been safely destroyed. Six of the eight continental chemical stockpiles, as well as the Johnson Atoll site, contained large numbers of assembled chemical weapons as well as bulk agent containers, while the other two continental sites stored only bulk agent containers. The demilitarization facilities that successfully dealt with both assembled weapons and bulk agent at five storage sites used several types of specialized furnaces to incinerate chemical agent and energetic materials and decontaminate metal munitions casings, bulk agent containers, and many agent-contaminated secondary waste streams. The two demilitarization facilities dealing only with bulk agent used chemical neutralization (aqueous-based hydrolysis) reactions to fragment and detoxify the chemical agents and a combination of decontamination solutions and steam to clean the agent containers. Demilitarization plants for the two remaining chemical weapons depots, which contain the remaining 10 percent of the nation's chemical agent in assembled chemical projectiles and rockets, are currently under construction. These facilities are funded separately under the DOD's Assembled Chemical Weapons Assessment (ACWA) program and implemented by a dedicated U.S. Army Element. Local concerns about incineration of chemical weapons forced the Army to design these facilities without the large furnaces used at other assembled chemical weapons demilitarization plants to destroy agent and energetics and to decontaminate many secondary waste materials. The lack of high-throughput furnaces to destroy or decontaminate secondary waste materials creates a need to easily and reliably determine which waste materials are contaminated with agent and if initial decontamination efforts have succeeded. Demilitarization facility closure activities might also be expedited if tools, equipment, and building surfaces could be monitored easily and reliably for agent contamination. While the Army has developed and successfully used methods to detect chemical agent contamination of various materials, these tend to be indirect and time consuming. Recent advances in analytical instrumentation suggest that it may be feasible to deploy robust portable instruments that can detect and characterize chemical agent contamination vii

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viii PREFACE of a wide variety of materials in real time. Formed under the auspices of the Board on Army Science and Technology (BAST), the Committee on Assessment of Agent Monitoring Strategies for the Blue Grass and Pueblo Chemical Agent Destruction Pilot Plants (ACWA Monitoring Committee) was appointed by the National Research Council to survey the capabilities of newly available analytical instrumentation, and to assess how such capabilities might be deployed to better characterize chemical agent contamination of secondary waste materials during agent destruction operations and provide a real-time monitoring tool for contaminated equipment and construction materials during closure activities at the last two U.S. chemical weapons stockpile demilitarization facilities. In the present report, the ACWA Monitoring Committee presents its findings and recommendations to the Program Manager for Assembled Chemical Weapons Alternatives (PMACWA), whose staff is responsible for the construction, operation, and closure of the last two U.S. chemical weapons stockpile demilitarization facilities. During its deliberations, the committee benefited from the insights and analyses of senior ACWA personnel and wishes to specifically acknowledge detailed inputs about anticipated ACWA operational procedures and requirements from C.J. Anderson and J.M. Kiley. The committee also benefited greatly from the efforts of BAST's professional staff, including the study director, Harrison T. Pannella, senior research associate Nia D. Johnson, and research assistant and logistics expert Ann F. Larrow. Charles E. Kolb, Chair Committee on Assessment of Agent Monitoring Strategies for the Blue Grass and Pueblo Chemical Agent Destruction Pilot Plants

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Acknowledgment of Reviewers This report has been reviewed in draft form by individuals chosen for their diverse perspectives and technical expertise, in accordance with procedures approved by the National Research Council's (NRC's) Report Review Committee. The purpose of this independent review is to provide candid and critical comments that will assist the institution in making its published report as sound as possible and to ensure that the report meets institutional standards for objectivity, evidence, and responsiveness to the study charge. The review comments and draft manuscript remain confidential to protect the integrity of the deliberative process. We wish to thank the following individuals for their review of this report: Charles K. Bayne, Consultant; John I. Brauman, NAS, Stanford University; Robert B. Cody, JEOL USA, Inc.; R. Graham Cooks, Purdue University; Gary S. Groenewold, Idaho National Laboratory; M. Douglas LeVan, Vanderbilt University; Fred W. McLafferty, NAS, Cornell University; W. Leigh Short, Consultant (retired); and G. Geoffrey Vining, Virginia Tech. Although the reviewers listed above have provided many constructive comments and suggestions, they were not asked to endorse the conclusions or recommendations nor did they see the final draft of the report before its release. The review of this report was overseen by Hyla S. Napadensky, Napadensky Energetics Inc. (retired). Appointed by the NRC, she was responsible for making certain that an independent examination of this report was carried out in accordance with institutional procedures and that all review comments were carefully considered. Responsibility for the final content of this report rests entirely with the authoring committee and the institution. ix

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Contents EXECUTIVE SUMMARY 1 1 INTRODUCTION 5 Report Motivation, 5 Committee Composition, 7 Committee Statement of Task, 7 Committee Activities, 8 Report Road Map, 9 2 BGCAPP AND PCAPP DESIGNS AND RELEVANT PROCEDURES USED AT DESTRUCTION FACILITIES 11 Background on Safety Procedures and Requirements Used at Chemical Agent Destruction Facilities, 12 Pueblo Chemical Agent Destruction Pilot Plant, 19 Blue Grass Chemical Agent Destruction Pilot Plant, 24 M55 Rocket Processing, 24 Projectile Processing, 29 Description of the HVAC Systems Used at Both Facilities, 29 3 AGENT MONITORING PRACTICES FOR WASTE GENERATED AT BGCAPP AND PCAPP 35 Waste Analysis Overview, 35 Waste Generation and Monitoring Overview, 36 Monitoring Based on Vapor Measurements, 43 Air Monitoring Instrumentation and Methods, 43 Extractive Analysis, 44 Use of DPE Suits During Plant Operations, 45 Changeover of Agent Disposal Campaigns at BGCAPP, 50 Closure Operations, 51 Activated Carbon Disposal, 56 Scenarios Summary, 57 xi

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xii CONTENTS 4 CURRENT STATUS OF SURFACE MEASUREMENT TECHNOLOGIES AND POTENTIAL ACWA SITE APPLICATIONS 59 Introduction, 59 Properties of the Target Molecules Relevant to Their Detection by Ambient Mass Spectrometry, 62 Experimental Methods for Ambient Mass Spectrometry, 68 Direct Analysis in Real Time (DART), 70 Desorption Electrospray Ionization (DESI), 80 Nonproximate Analysis by Ambient Mass Spectrometry, 82 Potential Roles for Ambient Mass Spectrometry in the ACWA Program, 87 Findings and Recommendations, 90 5 STATISTICAL METHODS AND MEASUREMENT 95 Overview, 95 Review of Existing Agent Measurement Approaches, 97 Analytical Measurement Issues, 98 Calibration Designs, 99 CWA Data Analysis Example, 100 Compliance Monitoring, 103 Statistical Sampling Issues, 104 Measurement Bias, Precision, and Detection Limits, 104 Measurement Basis, 105 Spatial Modeling, 106 Sampling Plans for Spatial Modeling, 108 Hot Spot Detection, 110 Sampling Plans for Hot Spot Detection, 111 6 REPORT SUMMATION AND RECOMMENDATIONS 113 Findings and Recommendations, 114 Conclusions, 123 REFERENCES 125 APPENDIXES A Biographical Sketches of Committee Members 137 B Committee Meetings 143 C Commercial Sources of Ambient Ionization Mass Spectrometry Instrumentation 147 D Statistical Calibration 151 E Sampling Variability and Uncertainty Analyses 163

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Tables, Figures, and Boxes TABLES 2-1 Processes and Unit Operations Being Used at PCAPP and BGCAPP, 13 2-2 Airborne Exposure Limits, Vapor Screening Levels, and Acute Exposure Guideline Levels for Chemical Agents, 14 2-3 Release Levels, Based on AEL Values, for Reuse of Items, 15 2-4 Room Contamination Requirements Using Near-Real-Time Monitoring of the Vapors in the Room, 18 2-5 Chemical Weapons Stockpile of HD- or HT-Filled Munitions at Pueblo Chemical Depot, 20 2-6 Description of the Chemical Weapons in the BGAD Stockpile, 25 3-1 Projected Amounts of Mustard-Agent-Contaminated Secondary Waste from Normal Operations at PCAPP, 38 3-2 Projected Amounts of Mustard-Agent-Contaminated Secondary Waste from Closure at PCAPP, 39 3-3 Projected Secondary Waste Streams for >1 VSL Agent-Contaminated Waste During Operations and Closure at BGCAPP, 40 3-4 Projected Secondary Waste Streams for <1 VSL Agent-Contaminated Waste During Operations and Closure at BGCAPP, 41 3-5 Estimated Agent-Contaminated Waste Stream Summary for Operations and Closure at BGCAPP, 42 3-6 Critical Measurement Performance Criteria for Possible Scenarios, 57 4-1 Physical Properties of Chemical Warfare Agents, 66 4-2 List of Acronyms (Ordered Alphabetically) and Relevant References Describing Various Ambient Surface Sampling Techniques, 69 4-3 Capabilities and Limitations of Ambient Mass Spectrometry (DART and DESI) and Existing Vapor Monitoring (DAAMS and MINICAMS) Measurement Strategies, 89 4-4 Comparative Capabilities and Limitations of DART and DESI for Characterization of Contamination by ACWA-Relevant Chemical Agents (GB, VX, HD), 90 xiii

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xiv TABLES, FIGURES, AND BOXES FIGURES 2-1 PCAPP munitions process flow chart, 21 2-2 Process and waste stream diagram for PCAPP, 22 2-3 PCAPP site layout, 23 2-4 BGCAPP munitions process flow chart, 24 2-5 Process and waste stream diagram for BGCAPP, 26 2-6 BGCAPP site layout, 27 2-7 The nine activated carbon filter units for the MDB HVAC system, 31 2-8 Vestibule on the side of an MDB HVAC unit, 31 2-9 Schematic representation of airflow through the six filter banks that make up each MDB filter unit, 32 2-10 A filter tray, 32 2-11 Airflow path through a filter tray, 33 3-1 An overview of the analysis plan for PCAPP, 46 3-2 Workers in personal protective equipment working at a chemical weapons disposal facility, 48 3-3 An example of a large item tented for monitoring at closure, 54 4-1 Schematic diagram of DART ion source, 61 4-2 Schematic diagram of DESI ion source, 61 4-3 Schematic illustrations showing the operation of several different ion sources and sampling schemes for ambient mass spectrometry, 71 4-4 Additional illustrations showing the operation of several different ion sources and sampling schemes for ambient mass spectrometry, 72 4-5 Laser-based ambient ionization techniques: (left) Laser Ablation-Electrospray Ionization (LAESI) and (right) Infrared Laser Ablation Metastable-induced Chemical Ionization (IR-LAMICI), 73 4-6 Schematic illustrations (this page and facing page) showing the operation of several different ion sources and sampling schemes for ambient mass spectrometry, 75 4-7 DART mass spectra of agent standards, 78 4-8 Structures of HD, GA, GB, and VX, with CAS designations in brackets, 79 4-9 High-resolution mass spectra obtained by DART for 800 ng VX on aluminum, concrete, and a bird feather, 79 4-10 Surfaces of steel, rubber hose, concrete, and charcoal spiked with 10 ng GB (top row) and unspiked surfaces (bottom row), 80 4-11 DESI remote sampling techniques, 84 4-12 DESI remote sampling techniques using AE and AFAI, 85 4-13 RASTIR and ND-EESI schematics, 85 4-14 Multiple-sprayer and nonproximate large-area sprayer DESI setups, 86 5-1 Estimated calibration function for VX in DI (deionized) water, 101

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TABLES, FIGURES, AND BOXES xv 5-2 Estimated relationship between variability and concentration for VX in DI (deionized) water, 101 5-3 Relationship between the percent relative standard deviation (%RSD) and concentration for VX in DI (deionized) water, 102 BOXES 2-1 Definition of Generator Knowledge, 33 3-1 Scenario 3A: Improving Worker Safety During DPE Entries, 49 3-2 Scenario 3B: Enabling More Efficient DPE Entries, 50 3-3 Definition and Classification of Occluded Spaces, 52 3-4 Scenario 3C: Process Area Occluded Space Surveys and/or Absorbed Agent Surveys During Changeover or Closure Activities, 53 3-5 Scenario 3D: Complex Contaminated Demilitarization Machine Needs Decontamination at Agent Changeover or Closure Activities, 53 3-6 Scenario 3E: Concrete Waste Contamination Evaluation, 56 3-7 Scenario 3F: Spent Activated Carbon Contamination Evaluation, 56

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Acronyms and Abbreviations AAS atomic absorption spectrometry ACS agent collection system ACWA Assembled Chemical Weapons Alternatives AEGLS acute exposure guideline levels AEL airborne exposure limit AFAI air flow assisted ionization ALT Acquisitions, Logistics & Technology ANCDF Anniston Chemical Agent Disposal Facility ANR agent neutralization reactor ANS agent neutralization system APB agent processing building APCI atmospheric pressure chemical ionization BGAD Blue Grass Army Depot BGCAPP Blue Grass Chemical Agent Destruction Pilot Plant BRAC base realignment and closure CAM cavity access machine CDC Centers for Disease Control and Prevention CDPHE Colorado Department of Public Health and the Environment CLLE continuous liquid-liquid extraction CMA Chemical Materials Agency (U.S. Army) CWA chemical warfare agent CWC Chemical Weapons Convention DAAMS depot area air monitoring system(s) DART direct analysis in real time DESI desorption electrospray ionization DL detection limit DMMP dimethyl methylphosphonate DPE demilitarization protective ensemble EBH energetics batch hydrolyzer ECR explosive containment room ECV explosion containment vestibule xvii

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xviii ACRONYMS AND ABBREVIATIONS EDT explosive destruction technology ENR energetics neutralization reactor EPA Environmental Protection Agency EQL expected quantitation limit ERB enhanced reconfiguration building ESI electrospray ionization ESSI electrosonic spray ionization FOAK first-of-a-kind [equipment] GB a nerve agent (sarin) GC-MS gas chromatography-mass spectrometry GPL general population limit H mustard agent HD distilled mustard agent HT distilled mustard mixed with bis(2-chloroethylthioethyl) ether HVAC heating, ventilation, and air conditioning ICB immobilized cell bioreactor ICP-MS inductively coupled plasma mass spectrometry IDLH immediately dangerous to life or health IP ionization potential JACADS Johnston Atoll Chemical Agent Disposal System LADESI laser ablation/desorption electrospray ionization LCL lower confidence limit LMQAP laboratory monitoring quality assurance plan LPMD linear projectile/mortar disassembly MCP monitoring concept plan MDB munitions demilitarization building MDL method detection limit MINICAMS miniature continuous air monitoring system(s) MPT metal parts treater MS mass spectrometry; mass spectrometer MSM munitions storage magazine MS/MS tandem mass spectrometry MTU munitions treatment unit MVUE minimum variance unbiased estimate MWS munitions washout system ND-EESI neutral desorption-extractive electrospray ionization NECDF Newport Chemical Agent Disposal Facility

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ACRONYMS AND ABBREVIATIONS xix NRC National Research Council OLS ordinary least squares OST occluded space team PCAPP Pueblo Chemical Agent Destruction Pilot Plant PCD Pueblo Chemical Depot PCE protective clothing and equipment PMACWA Program Manager for Assembled Chemical Weapons Alternatives PPE personal protective equipment PQL practical quantitation limit PVC polyvinyl chloride RASTIR remote analyte sampling, transport, and ionization relay RCM rocket cutting machine RCRA Resource Conservation and Recovery Act RD&D research development and demonstration SCWO supercritical water oxidation SFT shipping and firing tube SPME solid phase microextraction STEL short term exposure limit T chemical compound ((ClCH2CH2)2SCH2CH2)2O TAP toxological agent protective TCLP toxic characteristic leaching procedure TOC total organic carbon TOF time-of-flight TSDF treatment, storage and disposal facility UCL upper confidence limit UPL upper prediction limit VOC volatile organic compound VSL vapor screening level VX a nerve agent WAP waste analysis plan WCL waste control limit WLS weighted least squares

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