Abstract

Comparative estimation is performed for the repeatability of results from measuring the two main parameters (peak areas and retention times) of components (carbon dioxide, sulfur compounds) of a model mixture similar in composition to natural gas. The measurements are made on a capillary column prepared for the first time with nonpolar phase poly(1-trimethylsilyl-1-propyne) (PTMSP) with dimensions of 30 m × 0.53 mm and a sorbent film thickness of 2.82 μm, and a commercial Rt–Q–BOND column 30 m long and 0.32 mm in diameter, with a nonpolar polydivinylbenzene sorbent layer 10 μm thick. The use of these columns ensures satisfactory repeatability of the chromatographic characteristics of the analyzed compounds. The relative mean standard deviation (RMSD) for retention times is no greater than 0.10%. The RMSD for the measured peak areas is less than 1.92%. A slight difference between the peak areas for sulfur dioxide and carbon disulfide (five consecutive injections) is observed on an Rt-Q-BOND capillary column. The corresponding values of the RMSD are 4.22 and 2.52%. The magnitude of the signal response of the analyzed compounds is recorded with a microcatarometer. The limits for detecting sulfur-containing compounds on the PTMSP column change from 0.40 × 10⁻³ to 0.82 × 10⁻³ mg/mL. The possibility of selectively separating the macrozone of methane and the propane–butane fraction from trace hydrocarbons, sulfur compounds that contain carbon dioxide, hydrogen sulfide, and mercaptans on a capillary column with a film thickness of 2.82 μm PTMSP is also demonstrated for the first time.

中文翻译：

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非极性相多孔层毛细管柱上的轻烃和硫化合物的分析

摘要

通过测量组成类似于天然气的模型混合物的成分（二氧化碳，硫化合物）的两个主要参数（峰面积和保留时间），对结果的可重复性进行比较估计。测量是在毛细管柱上进行的，该毛细管柱首次使用非极性相聚（1-三甲基甲硅烷基-1-丙炔）（PTMSP）制备，尺寸为30 m×0.53 mm，吸附剂膜厚度为2.82μm，市售Rt –Q–BOND色谱柱长30 m，直径0.32 mm，非极性聚二乙烯基苯吸附剂层厚10μm。这些色谱柱的使用可确保所分析化合物的色谱特性具有令人满意的重复性。保留时间的相对平均标准偏差（RMSD）不大于0.10％。测量峰面积的RMSD小于1。92％。在Rt-Q-BOND毛细管柱上观察到二氧化硫和二硫化碳（连续5次进样）的峰面积之间存在细微差异。RMSD的相应值为4.22和2.52％。用微催化仪记录所分析化合物的信号响应幅度。PTMSP色谱柱上检测含硫化合物的极限从0.40×10更改^-3至0.82×10 ^-3 mg / mL。首次展示了在膜厚为2.82μmPTMSP的毛细管柱上选择性地从痕量烃，含二氧化碳，硫化氢和硫醇的痕量烃，甲烷和丙烷-丁烷馏分中分离出甲烷的大区域的可能性。 。