Department of Chemistry and Chemical Biology, Indiana University - Purdue University Indianapolis (IUPUI), 402 North Blackford Street LD326, Indianapolis, IN 46202, United States.
Department of Chemistry and Chemical Biology, Indiana University - Purdue University Indianapolis (IUPUI), 402 North Blackford Street LD326, Indianapolis, IN 46202, United States.
Talanta. 2019 Apr 1;195:580-586. doi: 10.1016/j.talanta.2018.11.060. Epub 2018 Nov 22.
Gas chromatography/mass spectrometry (GC/MS) is a "workhorse" instrument for chemical analysis, but it can be limited in its ability to differentiate structurally similar compounds. The coupling of GC to vacuum ultraviolet (VUV) spectroscopy is a recently developed technique with the potential for increased detection specificity. To date, GC/VUV has been demonstrated in the analysis of volatile organic compounds, petroleum products, aroma compounds, pharmaceuticals, illegal drugs, and lipids. This paper is the first to report on the utility of GC/VUV for explosives analysis in general, and the first to report on thermal degradation within the VUV cell and its analytical utility. The general figures of merit and performance of GC/VUV were evaluated with authentic standards of nitrate ester explosives (e.g., nitroglycerine (NG), ethylene glycol dinitrate (EGDN), pentaerythritol tetranitrate (PETN), and erythritol tetranitrate (ETN)). In addition, the explosive analytes were thermally degraded in the VUV cell, yielding reproducible, complex and characteristic mixtures of gas phase products (e.g., nitric oxide, carbon monoxide, and formaldehyde). The relative amounts of the degradation products were estimated via spectral subtraction of library spectra. Lastly, GC/VUV was used to analyze milligram quantities of intact and burned samples of double-base smokeless powders containing nitroglycerine, diphenylamine, ethyl centralite, and dibutylphthalate.
气相色谱/质谱联用（GC/MS）是化学分析的“主力仪器”，但在区分结构相似的化合物方面能力有限。GC 与真空紫外（VUV）光谱的耦合是一种最近开发的技术，具有提高检测特异性的潜力。迄今为止，GC/VUV 已在挥发性有机化合物、石油产品、香气化合物、药物、非法药物和脂质的分析中得到了证明。本文首次报道了 GC/VUV 一般用于爆炸物分析的实用性，以及首次报道了 VUV 池内的热降解及其分析实用性。使用硝酸酯炸药（例如硝化甘油（NG）、乙二醇二硝酸酯（EGDN）、季戊四醇四硝酸酯（PETN）和赤藓糖醇四硝酸酯（ETN））等真实标准评估了 GC/VUV 的一般质量和性能。此外，爆炸物分析物在 VUV 池内热降解，产生可重复、复杂且具有特征的气相产物混合物（例如，一氧化氮、一氧化碳和甲醛）。通过对库谱进行光谱减影，估算了降解产物的相对含量。最后，GC/VUV 用于分析含有硝化甘油、二苯胺、乙基中定剂和邻苯二甲酸二丁酯的双基无烟粉末的完整和燃烧样品的毫克量。
