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Committee to Assess Supercritical Water Oxidation System Testing for the Blue Grass Chemical Agent Destruction Pilot Plant Board on Army Science and Technology Division on Engineering and Physical Sciences

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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 Grant No. W911NF-13-1-0008 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:  978-0-309-28729-6 International Standard Book Number-10:  0-309-28729-4 Limited copies of this report are available from Additional copies are available from Board on Army Science and Technology The National Academies Press National Research Council 500 Fifth Street, NW 500 Fifth Street, NW, Room 940 Keck 360 Washington, DC 20001 Washington, DC 20001 (202) 334-3118 (800) 624-6242 or (202) 334-3313 http://www.nap.edu Copyright 2013 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. C. D. Mote 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 advis- ing 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 engineer- ing communities. The Council is administered jointly by both Academies and the Institute of Medicine. Dr. Ralph J. Cicerone and Dr. C. D. Mote are chair and vice chair, respectively, of the National Research Council. www.national-academies.org

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COMMITTEE TO ASSESS SUPERCRITICAL WATER OXIDATION SYSTEM TESTING FOR THE BLUE GRASS CHEMICAL AGENT DESTRUCTION PILOT PLANT JOHN R. HOWELL (NAE), Chair, University of Texas, Austin MARTIN A. ABRAHAM, Youngstown State University, Ohio DAVID J. DUQUETTE, Rensselaer Polytechnic Institute, Troy, New York ERIC M.V. HOEK, University of California, Los Angeles EVA K. LEE, Georgia Institute of Technology, Atlanta MURRAY GLENN LORD, Dow Chemical Company, Freeport, Texas JULIUS REBEK, JR. (NAS), Scripps Research Institute, La Jolla, California T.W. FRASER RUSSELL (NAE), University of Delaware, Newark PHILLIP E. SAVAGE, University of Michigan, Ann Arbor TIMOTHY SHEPODD, Sandia National Laboratories, Livermore, California Staff BRUCE BRAUN, Director, Board on Army Science and Technology JAMES C. MYSKA, Study Director DEANNA SPARGER, Program Administrative Coordinator 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, Arlington, Virginia ILESANMI ADESIDA, University of Illinois at Urbana-Champaign MARY E. BOYCE, Massachusetts Institute of Technology, Cambridge EDWARD C. BRADY, Strategic Perspectives, Inc., McLean, Virginia 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 H. HAMMOND, Independent Consultant, Fairfax, Virginia RANDALL W. HILL, JR., University of Southern California Institute for Creative Technologies, Playa Vista JOHN W. HUTCHINSON, Harvard University, Cambridge, Massachusetts 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, JVM LLC, Hampton, Virginia Staff BRUCE A. BRAUN, Director CHRIS JONES, Financial Associate DEANNA P. SPARGER, Program Administrative Coordinator vi

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Preface The United States joined the 1993 Convention on the than incineration) that could be used for the destruction of Prohibition of the Development, Production, Stockpiling and the lethal chemical agents that are associated with these Use of Chemical Weapons and on their Destruction (CWC) munitions.” The Army established a Program Manager for in April 1997. Under the CWC, the United States, along Assembled Chemical Weapons Assessment (PMACWA) to with 188 other states (as of 2012), agreed to eliminate their “identify and demonstrate not less than two alternatives to entire stockpiles of chemical weapons by April 2007. The the baseline incineration process for the demilitarization CWC allowed for one 5-year extension to this mandate, and of assembled chemical munitions.”1 Following a detailed the U.S. availed itself of this extension. Thus, the deadline selection process among proposed methods for destroying for full stockpile destruction was extended until April 2012. the weapons at Blue Grass Army Depot, PMACWA selected Over 90 percent of the U.S. stockpile of chemical agent and technologies using hydrolysis to destroy both agent and munitions had been disposed of by this extended deadline. Of energetic streams. The products of hydrolysis, called hydro- the nine stockpile sites, seven have completed agent destruc- lysate, are no longer as acutely toxic as the chemical agents. tion and the disposal facilities are either closed or undergoing At BGCAPP, the hydrolysates will be treated by super­critical closure. The Pueblo Chemical Agent Destruction Pilot Plant, water oxidation (SCWO) to further process them into envi- in Colorado, and the Blue Grass Chemical Agent Destruction ronmentally benign products. Pilot Plant (BGCAPP), in Kentucky, are being constructed This report discusses the results of the first-of-a-kind at the time of this writing to dispose of the remainder of the testing of the SCWO system. It also discusses the BGCAPP U.S. stockpile. response to the 2012 NRC report The Blue Grass Chemical Initially, the U.S. Army, following recommendations Agent Destruction Pilot Plant’s Water Recovery System and from the National Research Council (NRC), decided to use considers systemization of both the SCWO system itself incineration as its destruction method at all sites. Citizens in and the water recovery system. Finally, the report presents some states with stockpile storage sites opposed incineration fi ­ ndings and recommendations for systemization and testing because they believed it was impossible to determine the of these combined process elements. exact nature of the effluents escaping from the incineration I wish to express my gratitude to the members of the stacks. The Army pursued incineration at four of the eight Committee to Assess Supercritical Water Oxidation System storage sites in the continental United States. In response to Testing for the Blue Grass Chemical Agent Destruction growing public opposition to incineration, the Army devel- Pilot Plant. All members served as volunteers, and all have oped alternative processes to neutralize chemical agents by given unselfishly of their time and knowledge. The com- hydrolysis. These processes were used to destroy the VX mittee members’ expertise covered the needs of the project, nerve agent at Newport, Indiana, and the mustard agent at although most had a steep learning curve to assimilate the Aberdeen, Maryland. background and applications to chemical agent demilitariza- In 1996, public opposition to incineration in Kentucky tion. The members attended plenary meetings, toured the and Colorado caused Congress to enact Public Law 104-201, first-of-a-kind testing facility at General Atomics in San which instructed the Department of Defense to “conduct an Diego, California, toured the BGCAPP construction site, and assessment of the chemical demilitarization program for destruction of assembled chemical munitions and of the al- 1PMACWA has since been renamed the Program Executive Office, ternative demilitarization technologies and processes (other ACWA. vii

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viii PREFACE studied the extensive literature, including engineering charts their assistance. Meetings were arranged and run smoothly, and diagrams, provided to the committee by the technology and the committee was well cared for, in no small part due providers and the BGCAPP program staff. to the efforts of Deanna Sparger, the Program Administrative The committee recognizes and appreciates the extensive Coordinator for the Board on Army Science and Technology. support of the sponsor as well as the equipment contractors. I would like to acknowledge particularly the close working The committee also appreciates the openness and cordiality relationship I had with the NRC director for this study, James of the representatives of the technology providers. I believe Myska. Working as a team in leading this study, we were in our relationship with the sponsor, his team, and support close communication. contractors has been effective and constructive and that the committee has been given the best available information to John R. Howell, Chair conduct this evaluation. Committee to Assess Supercritical Water A study like this always requires extensive logistics Oxidation System Testing for the Blue Grass support, and the committee is indebted to the NRC staff for Chemical Agent Destruction Pilot Plant

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Acknowledgments This report has been reviewed in draft form by indi- Gerald S. Frankel, Ohio State University viduals chosen for their diverse perspectives and technical Keith P. Johnston, NAE, University of Texas expertise, in accordance with procedures approved by the Frederick J. Krambeck, NAE, ReacTech, Inc. National Research Council’s (NRC’s) Report Review Com- Digby D. MacDonald, University of California at mittee. The purpose of this independent review is to provide Berkeley candid and critical comments that will assist the institution Baoxia Mi, University of Maryland in making its published report as sound as possible and to Michael Schrage, Massachusetts Institute of Technology ensure that the report meets institutional standards for objec- tivity, evidence, and responsiveness to the study charge. The Although the reviewers listed above have provided many review comments and draft manuscript remain confidential to constructive comments and suggestions, they were not asked protect the integrity of the deliberative process. We wish to to endorse the conclusions or recommendations nor did thank the following individuals for their review of this report: they see the final draft of the report before its release. The review of this report was overseen by Hyla S. Napadensky, Robert A. Beaudet, Independent Consultant, Pasadena, Napadensky Energetics Inc. (retired). Appointed by the California National Research Council, she was responsible for making Madan M. Bhasin, NAE, Mid-Atlantic Technology, certain that an independent examination of this report was Research and Innovation Center carried out in accordance with institutional procedures and Andrew Brown, Jr., NAE, Delphi that all review comments were carefully considered. Respon- Richard A. Conway, NAE, Consultant, Atlantic Beach, sibility for the final content of this report rests entirely with Florida the authoring committee and the institution. ix

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Contents SUMMARY 1 1 INTRODUCTION 8 Stockpile Characteristics, 9 Overall BGCAPP Demilitarization Plan, 9 Description of the SCWO Process, 10 The Integrated SCWO/WRS System, 12 SCWO System Design and FOAK Test Objectives, 12 Statement of Task, 12 Report Overview, 13 References, 14 2 FIRST-OF-A-KIND TESTING 15 Integrated Operations, 15 Overview of Test Results, 16 Corrosion, 16 Elemental Sulfur Additive, 19 Variations in Feed Composition, 20 Functionality During FOAK Testing, 21 Maintainability, 23 References, 23 3 IMPLEMENTATION OF SUPERCRITICAL WATER OXIDATION AT BLUE GRASS 24 SCWO Feed Composition, 25 Safety, 26 Maintenance, 26 Process Exhaust, 27 Personnel Issues and Knowledge Transfer and Retention, 28 Effects of Aging and Storage on Component Operability, 28 SCWO Operations Manual for Interim Period, 29 Cyanide, 30 Overall System Operations and Computer Model, 31 References, 32 xi

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xii CONTENTS 4 SYSTEMIZATION OF THE SUPERCRITICAL WATER OXIDATION SYSTEM WITH THE WATER RECOVERY SYSTEM 33 Overview of the Water Recovery System, 33 2012 NRC Report on the BGCAPP Water Recovery System, 34 Key Concerns, 34 BGCAPP Response to the 2012 NRC Report, 35 Systemization of the WRS, 35 RO Membrane Storage After Systemization, 35 Development of Water Balance, 36 Impact of Water Recycling on the SCWO System, 36 Integrated SCWO and WRS Operations, 36 References, 37 APPENDIXES A Committee Activities 41 B Biographical Sketches of Committee Members 42

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Tables and Figures TABLES 2-1 Simulated Blended GB and Energetics Hydrolysates, 16 2-2 Simulated Blended VX and Energetics Hydrolysates, 16 2-3 Simulated Blended H and Energetics Hydrolysates, 16 2-4 Summary of Reported Maximum Average Corrosion Data Reported from FOAK Testing, 17 FIGURES S-1 Flow diagram of SCWO system and reverse osmosis WRS, 2 1-1  Simplified process diagram for the BGCAPP demilitarization process using hydrolysis f ­ ollowed by SCWO, 9 1-2 Program schedule for BGCAPP, 10 1-3  Phase diagram for water showing the operating conditions planned for the BGCAPP SCWO process, 11 1-4 Exterior view of the overall SCWO reactor, 11 1-5  Detailed drawing of the reactor showing the main parts of the reactor and how they are a ­ ssembled, where the feed nozzle enters the reactor, where the thermowells are placed in the reactor, and the process outlet from the reactor, 12 1-6 Flow diagram of SCWO system and reverse osmosis WRS, 13 3-1 SCWO block flow diagram showing only the SCWO system, 25 4-1 Flow of material from hydrolysis, through SCWO, up until the pretreatment step in the WRS, 34 4-2 Process flow diagram for the BGCAPP WRS, including the pretreatment and RO system, 34 xiii

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Acronyms and Abbreviations ACWA Assembled Chemical Weapons Alternatives NRC National Research Council BGCAPP Blue Grass Chemical Agent Destruction Pilot OWS oil-water separator Plant QDP quality data package CN− cyanide CWC Convention on the Prohibition of the RO reverse osmosis Development, Production, Stockpiling and Use of Chemical Weapons and on Their Destruction SCWO supercritical water oxidation FOAK first of a kind TDS total dissolved solids TOC total organic carbon GB a nerve agent, also known as sarin VX a nerve agent H a blistering agent, also known as mustard HCN hydrogen cyanide WRS water recovery system xiv