丙酮加氢产物气相色谱分析方法与技术的发展

E. Yakovleva, Mural Nurbol, G. A. Bukhtiyarova
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引用次数: 0

摘要

研究了不同固定相的毛细管色谱柱对丙酮加氢所得异丙醇纯度的测定能力。色谱柱为聚乙二醇20M,端接2-硝基对苯二甲酸(PEG20M/FFAP);保利(1-trimethylsilyl-1-propyne) (PTMSP032);和三氟丙基(25%)甲基有机硅弹性体(SKTFT 50X)。比较了测定时间、混合物组分的不对称系数(As)、丙酮/异丙醇和异丙醇/内标对化合物的分辨率(Rs),选择了PEG20M/FFAP毛细管柱。建立了用内标法测定丙酮和异丙醇气相质量分数的方法。正丁醇作为内标。丙酮的检出限为1.45,异丙醇的检出限为1.43,正丁醇的检出限为1.28·10 ~ 12 g/s。相对标准偏差(复发因子)在置信水平P = 0.95下未超过4.3%。
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Development of the Method and Technique to Analyze Acetone Hydrogenation Products by Gas Chromatography
Capillary chromatographic columns with different stationary phases were studied in order to compare their ability to estimate purity of isopropyl alcohol obtained by hydrogenation of acetone. The study was performed with the columns based on polyethylene glycol 20 M terminated with 2-nitroterephthalic acid (PEG20M/FFAP); poly(1-trimethylsilyl-1-propyne) (PTMSP032); and trifluoropropyl (25 %) methyl silicone elastomer (SKTFT 50X). A comparison of the measurement time, asymmetry factors (As) for components of the mixtures, and resolution (Rs) for the pairs of compounds acetone/isopropanol and isopropanol/internal standard gave grounds to choose a capillary column PEG20M/FFAP. A technique was developed for measuring the weight fractions of acetone and isopropanol using the method of internal standard in the gas phase. n-Butanol served as the internal standard. The detection limit was found to be 1.45 for acetone, 1.43 for isopropanol, and 1.28·10–12 g/s for n-butanol. Relative standard deviation (the recurrence factor) did not exceed 4.3 % at a confidence level P = 0.95.
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