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Consideration on the broad quantification range of gaseous reduced sulfur compounds with the combined application of gas chromatography and thermal desorber

机译:结合气相色谱法和热脱附器考虑气态还原硫化合物的宽定量范围

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In this work, the dynamic range of gas chromatography (GC) combined with a thermal desorber (TD) was investigated through a series of calibration experiments. To this end, standard gases of reduced sulfur compounds (RSC: H_2S, CH_3SH, DMS, CS_2 and DMDS) covering a relatively wide concentration range (2-100 nmol mol~(-1) (or ppb)) were analyzed by regulating sample loading range from 40 to 1200 mL (3.3-4900 pmol). It shows that the upper limits of GC-TD quantification are far higher than those of GC alone, although the cold trap unit in a TD suffers from breakthrough after a dose of RSC (e.g., 500 (DMDS) to 1600 pmol (H_2S)). Its quantification uncertainties tend to grow systematically with decreases in standard concentrations and sample loading volume, especially with H_2S. According to this study, the use of TD generally reduces the absolute detectability of GC by about one order of magnitude. Such reduction caused by TD application can be compensated efficiently with similar magnitude through the magnification of sample supply. Moreover, the TD system allows to increase sample volume (up to 3 orders of magnitude or above), it can ultimately help extend the practical range of RSC qualification in a fairly reliable manner.
机译:在这项工作中,通过一系列校准实验研究了气相色谱(GC)结合热脱附器(TD)的动态范围。为此,通过调节样品来分析涵盖相对较宽浓度范围(2-100 nmol mol〜(-1)(或ppb))的还原性硫化合物的标准气体(RSC:H_2S,CH_3SH,DMS,CS_2和DMDS)。上样量为40至1200 mL(3.3-4900 pmol)。结果表明,尽管在一定剂量的RSC(例如500(DMDS)至1600 pmol(H_2S))作用后,TD中的冷阱单元会出现突破,但GC-TD定量的上限远远高于单独的GC。 。随着标准浓度和样品上样量的减少,其定量不确定性趋于系统性增长,尤其是对于H_2S。根据这项研究,使用TD通常会使GC的绝对检测能力降低大约一个数量级。可以通过放大样品供应量,以类似的幅度有效补偿由TD应用引起的这种减少。此外,TD系统允许增加样品量(最多3个数量级或以上),最终可以以相当可靠的方式帮助扩展RSC鉴定的实用范围。

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