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首页> 外文期刊>Analytical and bioanalytical chemistry >Development and validation of a sensitive thermal desorption–gas chromatography–mass spectrometry (TD-GC-MS) method for the determination of phosgene in air samples
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Development and validation of a sensitive thermal desorption–gas chromatography–mass spectrometry (TD-GC-MS) method for the determination of phosgene in air samples

机译:灵敏的热脱附-气相色谱-质谱(TD-GC-MS)方法开发和验证,用于测定空气中的光气

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摘要

A new rapid, sensitive and reliable method was developed for the determination of phosgene in air samples using thermal desorption (TD) followed by gas chromatography– mass spectrometry (GC-MS). The method is based on a fast (10 min) active sampling of only 1 L of air onto a Tenax? GR tube doped with 0.5 mL of derivatizing mixture containing dimercaptotoluene and triethylamine in hexane solution. Validation of the TD-GC-MS method showed a low limit of detection (40 ppbv), acceptable repeatability, intermediate fidelity (relative standard deviation within 12 %) and excellent accuracy (>95 %). Linearity was demonstrated for two concentration ranges (0.04 to 2.5 ppmv and 2.5 to 10 ppmv) owing to variation of derivatization recovery between low and high concentration levels. Due to its simple on-site implementation and its close similarity with recommended operating procedure (ROP) for chemical warfare agents vapour sampling, the method is particularly useful in the process of verification of the Chemical Weapons Convention.
机译:开发了一种新的快速,灵敏和可靠的方法,通过热脱附(TD)然后气相色谱-质谱(GC-MS)测定空气样品中的光气。该方法基于对Tenax?上仅1 L空气的快速(10分钟)主动采样。 GR管中掺有0.5 mL含二巯基甲苯和三乙胺的己烷溶液衍生化混合物。 TD-GC-MS方法的验证显示出低检测限(40 ppbv),可接受的重复性,中等保真度(相对标准偏差在12%以内)和极佳的准确性(> 95%)。由于在低浓度水平和高浓度水平之间衍生化回收率的变化,证明了两个浓度范围(0.04至2.5 ppmv和2.5至10 ppmv)的线性。由于该方法简单易行,并且与化学战剂蒸气采样的推荐操作程序(ROP)相似,因此在验证《化学武器公约》的过程中特别有用。

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