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Tuneable Microsecond-Pulsed Glow Discharge Design for the Simultaneous Acquisition of Elemental and Molecular Chemical Information Using a Time-of-Flight Mass Spectrometer

机译:可调谐微秒脉冲辉光放电设计,用于使用飞行时间质谱仪同时获取元素和分子化学信息

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摘要

A microsecond-pulsed direct current glow discharge (GD) was interfaced and synchronized to a time-of-flight mass spectrometer MS(TOF) for time-gated generation and detection of elemental, structural, and molecular ions. In this way, sequential collection of the mass spectra at different temporal regimes occurring during the GD pulse cycle is allowed. The capabilities of this setup were explored using bromochloromethane as model analyte. A simple GD chamber, developed in our laboratory and characterized by a low plasma volume minimizing dilution of the sample but showing great robustness to the entrance of organic compounds in the microsecond-pulsed plasma, has been used. An exhaustive analytical characterization of the GD-MS(TOF) prototype has been performed. Calibration curves for bromochloromethane observed at the different time regimes of the GD pulse cycle (that is, for elemental, fragment, and molecular ions from the analyte) showed very good linearity for the measurement of the different involved ions, with precisions in the range of 7-13percent (relative standard deviation). Actual detection limits obtained for bromochloromethane were in the range of 1-3 (mu)g/L for elements monitoring in the GD pulse "prepeak", in the range of 11-13 (mu)g/L when monitoring analyte fragments in the plateau, and about 238 (mu)g/L when measuring the molecular peak in the afterpeak regime.
机译:微秒脉冲直流辉光放电(GD)连接并同步到飞行时间质谱仪MS(TOF),用于在时间选通时生成和检测元素,结构和分子离子。以这种方式,允许在GD脉冲周期期间在不同的时间范围内依次收集质谱。使用溴氯甲烷作为模型分析物探索了此设置的功能。我们使用了一个简单的GD腔室,该腔室是由我们的实验室开发的,具有低血浆量,最大程度地减少了样品的稀释,但对微秒脉冲血浆中有机化合物的入口显示出强大的鲁棒性。已经对GD-MS(TOF)原型进行了详尽的分析表征。在GD脉冲周期的不同时间范围内(即来自分析物的元素,碎片和分子离子)观测到的溴氯甲烷的校准曲线显示出非常好的线性,可用于测量不同的所涉及离子,其精确度范围为7-13%(相对标准偏差)。对于GD脉冲“前峰”中的元素监测,对溴氯甲烷的实际检测限在1-3μg/ L的范围内,而在监测样品中的分析物碎片时,则在11-13μg/ L的范围内。峰,在后峰状态下测量分子峰时约为238μg/ L。

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