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A Portable, High-Speed, Vacuum-Outlet GC Vapor Analyzer Employing Air as Carrier Gas and Surface Acoustic Wave Detection

机译:便携式,高速,真空出口气相色谱气相分析仪,利用空气作为载气和表面声波检测

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Vacuum-outlet GC with atmospheric-pressure air as the carrier gas is implemented at outlet pressures up to 0.8 atm using a low-dead-volume polymer-coated surface acoustic wave (SAW) detector. Increases in the system outlet pressure from 0.1 to 0.8 atm lead to proportional increases in detector sensitivity and significant increases in column efficiency. The latter effect arises from the fact that optimal carrier gas velocities are lower in air than in more conventional carrier gases such as helium or hydrogen due to the smaller binary diffusion coefficients of vapors in air. A 12-m-long, 0.25-mm-i.d. tandem column ensemble consisting of 4.5-m dimethyl polysiloxane and 7.5-m trifluoropropylmethyl polysiloxane operated at an outlet pressure of 0.5 atm provides up to 4×10~(4) theoretical plates and a peak capacity of 65 (resolution, 1.5) for a 3-min isothermal analysis. At 30℃, mixtures of vapors ranging in vapor pressure from 8.6 to 76 Torr are separated in this time frame. The SAW detector cell has an internal volume of <2 μL, which allows the use of higher column outlet pressures with minimal dead time. The sensor response is linear with solute mass over at least 2-3 decades and provides detection limits of 20-50 ng for the vapors tested. The combination of atmospheric-pressure air as carrier gas, modest operating pressures, and SAW sensor detection is well-suited for field instrumentation since it eliminates the need for support gases, permits smaller, low-power pumps to be used, and provides sensitivity to a wide range of vapor analytes.
机译:使用低死体积聚合物涂层的表面声波(SAW)检测器,在出口压力高达0.8 atm的压力下,实现了以大气压空气为载气的真空出口GC。系统出口压力从0.1 atm增加到0.8 atm,导致检测器灵敏度成比例增加,并且色谱柱效率显着提高。后一种效果来自以下事实:由于空气中蒸气的二元扩散系数较小,因此最佳载气在空气中的速度低于更传统的载气(例如,氦气或氢气)。长度为12米,内径为0.25毫米由4.5米的二甲基聚硅氧烷和7.5米的三氟丙基甲基聚硅氧烷组成的串联色谱柱色谱柱,在0.5 atm的出口压力下运行,可提供高达4×10〜(4)个理论塔板和3个色谱柱的峰容量为65(分辨率1.5) -min等温分析。在此温度范围内,在30℃时,分离出蒸气压范围为8.6至76 Torr的蒸气混合物。 SAW检测器池的内部体积小于2μL,从而可以使用较高的色谱柱出口压力,而使死区时间最短。传感器响应至少在2-3年内与溶质成线性关系,并且对测试的蒸汽提供20-50 ng的检测极限。大气压空气作为载气,适中的工作压力以及SAW传感器检测的组合非常适合现场仪表,因为它消除了对辅助气体的需求,允许使用较小的低功率泵,并且对各种各样的蒸气分析物。

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