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DART-MS analysis of inorganic explosives using high temperature thermal desorption

机译:使用高温热脱附的DART-MS分析无机炸药

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摘要

An ambient mass spectrometry (MS) platform coupling resistive Joule heating thermal desorption (JHTD) and direct analysis in real time (DART) was implemented for the analysis of inorganic nitrite, nitrate, chlorate, and perchlorate salts. The resistive heating component generated discrete and rapid heating ramps and elevated temperatures, up to approximately 400 °C s−1 and 750 °C, by passing a few amperes of DC current through a nichrome wire. JHTD enhanced the utility and capabilities of traditional DART-MS for the trace detection of previously difficult to detect inorganic compounds. A partial factorial design of experiments (DOE) was implemented for the systematic evaluation of five system parameters. A base set of conditions for JHTD-DART-MS was derived from this evaluation, demonstrating sensitive detection of a range of inorganic oxidizer salts, down to single nanogram levels. DOE also identified JHTD filament current and in-source collision induced dissociation (CID) energy as inducing the greatest effect on system response. Tuning of JHTD current provided a method for controlling the relative degrees of thermal desorption and thermal decomposition. Furthermore, in-source CID provided manipulation of adduct and cluster fragmentation, optimizing the detection of molecular anion species. Finally, the differential thermal desorption nature of the JHTD-DART platform demonstrated efficient desorption and detection of organic and inorganic explosive mixtures, with each desorbing at its respective optimal temperature.
机译:结合电阻式焦耳加热热脱附(JHTD)和实时直接分析(DART)的环境质谱(MS)平台用于分析无机亚硝酸盐,硝酸盐,氯酸盐和高氯酸盐。电阻加热组件通过使几安培的直流电流通过一条镍铬合金导线,从而产生了离散且快速的加热斜坡和升高的温度,最高达到约400°C s -1 和750°C。 JHTD增强了传统DART-MS的痕量检测以前难以检测的无机化合物的实用性和功能。实验的部分析因设计(DOE)用于对五个系统参数进行系统评估。从该评估中得出了JHTD-DART-MS的基本条件集,表明灵敏地检测了一系列无机氧化剂盐,甚至低至单纳克水平。 DOE还确定了JHTD灯丝电流和源内碰撞诱导解离(CID)能量对系统响应的影响最大。 JHTD电流的调谐提供了一种控制热脱附和热分解相对程度的方法。此外,源内CID还提供了加合物和簇碎片的操作,优化了分子阴离子种类的检测。最后,JHTD-DART平台的不同热脱附性质证明了有机和无机炸药混合物的有效脱附和检测,每种脱附均在其各自的最佳温度下进行。

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