Fast GC-PFPD system for field analysis of chemical warfare agents

Gad Frishman, Aviv Amirav
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引用次数: 34

Abstract

A fast gas chromatograph (GC) equipped with a pulsed-flame photometric detector (PFPD) was designed and built with the intention of facilitating field analysis of the full range of chemical warfare agents (CWA). This GC-PFPD system was tested with five organophosphorus and organosulfur CWA simulants that cover the volatility range of common CWA. Fast repetitive analysis was demonstrated with a cycle time as short as 30 s, combined with very low detection limits of 20 ng/m3 for organophosphorus CWA simulants and 200 ng/m3 for organosulfur compounds. With a longer analysis time of 80 s, a 3-ng/m3 detection limit was demonstrated for DMMP. In the GC-PFPD system, the separation power of each of these techniques is orthogonal and independent; thus, this hyphenated combination is characterized by a very low false-alarm rate, combined with CWA identification capability at the molecular level. The large improvement in system selectivity is demonstrated in the direct analysis of a low level of triethylphosphate in the headspace of diesel fuel without any interference. The system inlet was heated and the sample path was inert without any metal, enabling fast response time and low detection limits for a low volatility agent such as VX. The same fast GC-PFPD system could also be quickly and easily switched to a continuous sampling “sniff” mode of operation with 2-s response time. Alternatively, it could be operated in a novel mode of thermally modulated inlet (TMI) that provided intermediate results between those of GC and “sniff” in terms of the trade-off of response time and performance. The fast GC-PFPD system is also characterized by low average hydrogen consumption (about 4 ml/min), small size, and low weight. No attempt was made to complete the system in terms of portable control electronics. The advantages and unique features of this system, as well as the importance of CWA identification at the molecular level, are discussed. © 2000 John Wiley & Sons, Inc. Field Analyt Chem Technol 4: 170–194, 2000

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用于化学战剂现场分析的快速GC-PFPD系统
设计并研制了一种配备脉冲火焰光度检测器(PFPD)的快速气相色谱仪(GC),以方便对全系列化学战剂(CWA)的现场分析。用五种有机磷和有机硫CWA模拟剂对GC-PFPD系统进行了测试,这些模拟剂覆盖了普通CWA的挥发性范围。快速重复分析证明,周期时间短至30秒,结合极低的检测限,有机磷CWA模拟物为20 ng/m3,有机硫化合物为200 ng/m3。分析时间较长,为80 s, DMMP的检出限为3 ng/m3。在GC-PFPD系统中,这两种技术的分离功率相互正交且相互独立;因此,这种连字符组合具有非常低的误报率,并具有分子水平上的CWA识别能力。在柴油顶空中无任何干扰地直接分析低水平的三乙基磷酸,证明了系统选择性的大幅度提高。系统入口被加热,样品路径是惰性的,不含任何金属,对VX等低挥发性试剂具有快速响应时间和低检测限。同样的快速GC-PFPD系统也可以快速轻松地切换到连续采样“嗅探”模式,响应时间为2秒。或者,它可以在一种新的热调制入口(TMI)模式下运行,该模式在响应时间和性能的权衡方面提供介于GC和“嗅探”之间的中间结果。快速GC-PFPD系统还具有平均耗氢量低(约4 ml/min)、体积小、重量轻的特点。没有尝试在便携式控制电子设备方面完成该系统。讨论了该系统的优点和独特之处,以及在分子水平上进行水化学反应鉴定的重要性。©2000 John Wiley &儿子,Inc。化学工程学报(自然科学版),2004,31 (4):393 - 394
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