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1
Introduction
REPORT MOTIVATION
During the middle third of the twentieth century, the United States developed and
produced a wide range of weapons designed to disperse both nerve (GB and VX) and
blister (sulfur mustard: H, HD, and HT) chemical agents at lethal concentrations.
Although never used, 31,496 tons of chemical agents were produced after World War II,
a large fraction of which was loaded into millions of individual munitions, with the rest
stored in bulk containers. The agent-filled munitions and bulk containers that remained in
the United States were stored in eight continental weapons depots, while chemical
munitions that had been sent overseas were consolidated and stored on Johnson Atoll,
southwest of the main Hawaiian islands.
In 1985, Congress directed the U.S. Army to start destruction of some elements in
the chemical weapons stockpile (Public Law 99-145), and in 1991 Congress directed that
all chemical weapons be destroyed (Public Law 102-484). In 1997 Congress ratified the
Chemical Weapons Convention (CWC), an international treaty that specified all chemical
weapons would be destroyed by April 29, 2012. What is now the Army's Chemical
Materials Agency (CMA) has built and operated chemical agent disposal facilities at
Johnson Atoll and six of the eight continental U.S. storage depots, successfully
destroying the agent-filled munitions and/or agent in bulk containers at all seven CMA
sites. These activities have successfully destroyed 90 percent of the nation's stockpiled
chemical agents.
Congress assigned the job of destroying the stockpiled chemical weapons at the
two remaining continental U.S. depots (in Lexington, Kentucky, and Pueblo, Colorado)
to a separate U.S. Army Element, the Assembled Chemical Weapons Alternatives
(ACWA) organization. This occurred after residents near these two facilities convinced
their congressional representatives that they were seriously concerned about the safety
and effectiveness of CMA's technology selection for assembled weapons, based on
robotic disassembly and separate incineration of the chemical agent and energetic
materials in agent-filled munitions. The time required to define, assess, and develop
alternative assembled weapons demilitarization technologies, coupled with serious
budget constraints, has delayed chemical weapons destruction at Lexington and Pueblo;
their demilitarization plants are still under construction.
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6 ASSESSMENT OF AGENT MONITORING STRATEGIES FOR BGCAPP AND PCAPP
All chemical weapon demilitarization technologies generate large amounts of
potentially agent-contaminated secondary wastes as well as contaminated equipment,
machinery, and plant structural elements. Chemical agent contamination levels for
secondary waste, process machinery, and demilitarization equipment (tools, respirators,
instruments, etc.) resulting from agent and energetics destruction processes have to be
determined in order to develop safe decontamination strategies and/or disposal options.
Furthermore, demilitarization plant structural elements may need to be decontaminated
for maintenance activities required during disposal operations and agent changeover
breaks in plant operations and during plant closure.
CMA has developed methods for determining whether waste materials,
equipment, machinery, and even structural elements are contaminated by chemical
agents. These methods generally involve (1) isolating the objects of interest in some sort
of enclosure and (2) after a specified equilibration time, measuring vaporized agent
concentrations in the enclosure's headspace. In other cases, wipe samples of surfaces can
be obtained and solvents may be used to extract chemical agent contaminants from wipe
samples or waste stream materials and then analyzed with chromatographic techniques.
These proven techniques are available and are planned for use in the two new ACWA
demilitarization plants now being built.
While effective, these traditional methods can be time consuming and have to be
repeated if initial decontamination efforts are not successful. A recent review, focused on
technologies for quantifying agent vapor concentrations in CMA demilitarization
facilities (NRC, 2005a), noted the potential of then newly developed ambient surface
ionization mass spectrometry techniques to provide real-time measurements of chemical
agent contamination on surfaces. Ambient ionization mass spectrometry involves
sampling and ionization of chemical species in their native environment without, or with
minimal, sample preparation. Objects sampled are usually solids, and the experiment is
typically done at atmospheric pressure, with total analysis times on the order of a few
seconds. Subsequent development of a wide range of ambient surface ionization
techniques with mass spectrometric detection has been rapid and impressive. Significant
improvements in sensitivity, response time, portability, and reliability have been
demonstrated, and an increasing number of systems are or will soon be commercially
available.
This study is focused on whether ambient surface ionization analytical techniques
are sufficiently sensitive, specific, rapid, robust, and available to supplement current
Army methods for screening materials, equipment, and structural elements for agent
contamination. Considerable time and effort are spent characterizing and
decontaminating secondary waste, process machinery, and equipment during both
disposal operations and plant closure; this significantly extends the time needed for safe
and effective chemical weapons destruction and prolongs plant closure. If robust,
portable, real-time surface agent contamination analytical instrumentation is available
and can shorten the time and effort required for tasks not directly contributing to
chemical weapons destruction, they may be well worth deploying at the two new ACWA
demilitarization plants.
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INTRODUCTION 7
COMMITTEE COMPOSITION
The Committee on Assessment of Agent Monitoring Strategies for the Blue Grass
and Pueblo Chemical Agent Destruction Pilot Plants (or ACWA Monitoring Committee)
is made up of experts on analytical chemistry (including mass spectrometry and ion
mobility measurements), plasma chemistry, environmental chemistry, environmental
engineering, statistical sampling and experimental design, process chemical engineering,
materials science, quantitative risk assessment, industrial engineering, and environmental
regulations. Short biographies of the committee members are presented in Appendix A.
COMMITTEE STATEMENT OF TASK
The committee's statement of task is as follows:
The Program Manager for Assembled Chemical Weapons Alternatives
(PMACWA) is currently in the process of constructing two chemical agent
destruction facilities, the Blue Grass Chemical Agent Destruction Pilot Plant
(BGCAPP) in Richmond, Kentucky and the Pueblo Chemical Agent Destruction
Pilot Plant (PCAPP) in Pueblo, Colorado. According to the current plant design,
BGCAPP will dispose of mustard agent H, and nerve agents GB (sarin) and VX
using chemical neutralization followed by supercritical water oxidation and
PCAPP will dispose of mustard agent HD and HT, using chemical neutralization
followed by biotreatment. In addition, the selection of an auxiliary explosive
destruction technology (EDT) to handle leakers and reject munitions at PCAPP,
and exploration of the use of this type of technology to possibly process M55
rocket motors and mustard agent munitions at BGCAPP is currently being
investigated by ACWA.
Construction of BGCAPP and PCAPP is in the early stages and chemical agent
monitoring strategies have not yet been finalized for these facilities. PMACWA
will adopt monitoring methods for airborne agent at BGCAPP and PCAPP
similar to those used by the U.S. Army Chemical Materials Agency (CMA) at its
facilities. The current U.S. Army monitoring procedures have been considered to
be sound and proven. However, PMACWA could benefit from a National
Research Council (NRC) assessment of any technology advancements to monitor
for agent contamination of solid waste materials as well as facility equipment and
surfaces at BGCAPP and PCAPP using emerging technologies. Advancements in
real-time and near real-time monitoring technology for chemical agents, agent
simulants and similar semi-volatile chemicals are being regularly documented in
the scientific literature and may present opportunities to build additional
efficiencies into waste disposal and closure activities at BGCAPP and PCAPP.
The National Research Council will establish an ad hoc committee to:
Review the process designs for both BGCAPP and PCAPP to evaluate
the expected degree of contamination for facility solid wastes,
equipment, and surfaces anticipated from agent destruction processes.
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8 ASSESSMENT OF AGENT MONITORING STRATEGIES FOR BGCAPP AND PCAPP
Evaluate novel candidate technologies capable of real-time and near real-
time quantification of chemical agents adsorbed onto or absorbed into
materials relevant to chemical demilitarization operational and closure
processes and identify specifications required for a new monitoring
technology to improve BGCAPP and PCAPP waste disposal and plant
closure activities.
Using the specifications identified in bullet two, review and assess new
and emerging technologies that enable rapid measurement of the degree
of contamination of process equipment and waste, or if the degree of
decontamination achieved is sufficient to meet established regulatory
requirements, including requirements for off-site shipment of wastes.
Specifically, promising novel technologies will be evaluated for
detection and quantification of chemical agents adsorbed onto DPE suits,
agents absorbed into activated charcoal, and agents adsorbed onto and/or
absorbed into concrete surfaces.
COMMITTEE ACTIVITIES
The committee met in Aberdeen, Maryland (February 2011), Pueblo, Colorado
(June 2011), Washington, D.C. (August 2011), and Irvine, California (October, 2011).
Briefings on chemical demilitarization activities and technologies and ambient ionization
analytical techniques were presented by the following organizations:
Army Element Assembled Chemical Weapons Alternatives
Army Chemical Materials Agency
Army Edgewood Chemical Biological Center
Battelle Memorial Institute
Idaho National Laboratory
Purdue University, Department of Chemistry
At these meetings, committee members also went over technical details,
discussed, outlined, and wrote draft report sections, and reviewed report drafts.
Additional information on the committee's meetings is given in Appendix B.
Based on their respective expertise and experience, committee members were
assigned to one or more of four working groups. These groups performed the bulk of the
technical analyses and draft writing assignments. The four working groups were these:
Plant Processes
Current Waste and Structural Contamination Evaluation Practices
Analytical Technologies
Measurement Methodologies
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INTRODUCTION 9
REPORT ROAD MAP
Chapter 2 of this report describes the planned chemical weapons destruction
processes to be employed at the two ACWA demilitarization facilities and analyzes the
probable secondary waste streams and planned waste treatment and disposal activities.
Current Army methods for monitoring chemical agent contamination of secondary waste
materials as well as equipment, machinery, and structural components during agent
changeout and plant closure activities are first presented in Chapter 2 and then elaborated
on in Chapter 3. Chapter 3 also presents potential scenarios in which real-time surface or
condensed phase agent measurements might be useful. Chapter 4 reviews the current
state of the art of analytical ambient ionization mass spectrometry and discusses potential
analysis tasks and technology implementations. An analysis of statistical sampling design
methods and information on their application to chemical agent surface contamination
measurements in relevant chemical demilitarization plant scenarios are presented in
Chapter 5. The committee's findings and recommendations are compiled in Chapter 6. As
previously indicated, Appendix A contains short biographical sketches of the committee
members and Appendix B provides details of committee meeting activities. Appendix C
lists some known current sources of commercially available ambient ionization mass
spectrometry equipment in support of the technical presentation in Chapter 4. Appendix
D on statistical calibration and Appendix E on sampling variability and uncertainty
analyses supplement the statistical presentation in Chapter 5.
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