Indirect determination of O-ethyl S-(2-diisopropylaminoethyl) methylphosphonothioate in air at low concentrations
| Autor: | William K. Fowler, Josiah E. Smith |
|---|---|
| Rok vydání: | 1989 |
| Předmět: |
Detection limit
Analyte Sorbent Chromatography Chromatography Gas biology Chemistry Organic Chemistry Relative standard deviation Organothiophosphorus Compounds General Medicine Biochemistry Analytical Chemistry Silver fluoride biology.protein Gas chromatography Cholinesterase Inhibitors Volume concentration Cholinesterase |
| Zdroj: | Journal of chromatography. 478(1) |
| Popis: | This paper describes an indirect method for the quantification of the toxic military agent O-ethyl S-(2-diisopropylaminoethyl) methylphosphonothioate (VX) in the vapor state in air or other similar gases at ng/m 3 levels. The method begins with the passage of a gaseous sample through a filter impregnated with silver fluoride to convert the VX vapor to ethyl methylphosphonofluoridate. The latter compound is then trapped on a bed of Chromosorb 106, transferred to a smaller bed of the same sorbent, and desorbed thermally into a gas chromatograph equipped with a flame-photometric detector. The method is comparable in sensitivity to the principal alternative method, which is based on cholinesterase inhibition, and it is less subject to interference from common organic solvents and other cholinesterase inhibitors. The detection limit was found to be limited by, and therefore dependent on, the nature and extent of any background substances that produced a significant chromatographic signal or response at the retention time of the analyte. In the absence of such substances, the instrument provided a response to 0.19 ng of VX that was thirty times larger than the peak-to-peak noise amplitude on the chromatographic base line. Moreover, the method bias ( i.e. , 100% minus the percent VX recovery) was found to depend on VX concentration, with estimates of agent recovery ranging from 83% at a VX concentration of 0.67 ng/m 3 to 104% at a concentration of 0.084 ng/m 3 . The relative standard deviation varied with VX concentration and with the nature of the test that was performed to estimate it. It ranged from 2.1 % in one VX vapor-challenge test to 17% in an experiment involving spiked sampling tubes, and it was generally lower at the higher VX test concentrations. |
| Databáze: | OpenAIRE |
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