Quantitative methods have been developed for the analysis of chemical warfare agent degradation products in reaction masses using capillary electrophoresis (CE). This is the first report of a systematic validation of a CE-based method for the analysis of chemical warfare agent degradation products in agent neutralization matrixes (reaction masses). After neutralization with monoethanolamine/water, the nerve agent GB (isopropyl methylphosphonofluoridate, Sarin) gives isopropyl methylphosphonic acid (IMPA) and O-isopropyl O'-(2-amino)ethyl methylphosphonate (GB-MEA adduct). The nerve agent GD (pinacolyl methylphosphonofluoridate, Soman), [pinacolyl = 2-(3,3-dimethyl)butyl] produces pinacolyl methylphosphonic acid (PMPA) and O-pinacolyl O'-(2-amino)ethyl methylphosphonate (GD-MEA adduct). The samples were prepared by dilution of the reaction masses with deionized water before analysis by CE/indirect UV detection or CE/conductivity detection. Migration time precision was less than 4.0% RSD for IMPA and 5.0 RSD for PMPA on a day-to-day basis. The detection limit for both IMPA and PMPA is 100 micrograms/L; the quantitation limit for both is 500 micrograms/L. For calibration standards, IMPA and PMPA gave a linear response (R2 = 0.9999) over the range 0.5-100 micrograms/mL. The interday precision RSDs were 1.9, 1.0, and 0.7% for IMPA at 7.5, 37.5 and 75.0 micrograms/mL, respectively. Corresponding values for PMPA (again, RSD) were 2.9, 1.1, and 1.0% at 7.5, 37.5 and 87.5 micrograms/mL, respectively, as before. Analysis accuracy was assessed by spiking actual neutralization samples with IMPA or PMPA. For IMPA, the seven spike levels used ranged from 20 to 220% of the IMPA background level, and the incremental change in the found IMPA level ranged from 86 to 99 % of the true spiking increment (R2 = 0.9987 for the linear regression). For PMPA, the five spike levels ranged from 10 to 150% of the matrix background level, and similarly, the accuracy obtained ranged from 95 to 97% of the true incremental value (R2 = 0.9999 for the linear regression).

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The U.S. Department of Defense (DOD) has engaged in destroying the U.S. stockpile of chemical weapons under the convention that was signed on January 13, 1993 on the prohibition of development, production, stockpiling and use of chemical weapons, and on their destruction of chemical weapons. The Pueblo Chemical Agent-Destruction Pilot Plant (PCAPP) is designed and constructed to destroy chemical agents by hydrolysis at a chemical munitions disposal facility of the DOD in Pueblo, Colorado. The State of Colorado encourages recycling water and minimizing water usage to the extent practicable because of the water shortage in southern Colorado. The permitted capacity of the wells supplying the PCAPP water system is 218,800 gallons per day (gpd). Water usage above this level must be provided by additional sources. PCAPP water usage in summer is estimated to be approximately 60,000 gpd. PCAPP design uses Veolia Water evaporation and crystallization technologies to recover water from the biotreated effluent. More than 80% of the recovered water is used to dilute the hydrolysate for biotreatment. Approximately 103 gpm (148,000 gpd) biotreated effluent is evaporated to recover water for reuse at the site. PCAPP permit requires that the recovered water quality from the BRS is acceptable for use as an effective substitute for well water at the site. Therefore, the recovered water is processed through granular activated carbon (GAC) adsorption units to comply with the Maximum Concentration Levels (MCLs) listed in the National Primary Drinking Water Standards. This paper presents results from evaporation/crystallization, dewatering, and carbon adsorption tests to confirm performance to meet the design parameters. Material selection for high chloride content (4,000-5,000 mg/L), foaming resulting from biosolids, and organics removal from offgas were some of the design challenges.