甲醇气相氧化羰基化产物在线气相色谱分析

On-line GC Analysis of Products in the Synthesis of Dimethyl Carbonate by Vapor-Phase Oxidative Carbonylation of Methanol

采用三阀四柱多维毛细管气相色谱对甲醇气相氧化羰基化合成碳酸二甲酯的产物进行在线一次分析。采用了标准物质对照法对产物中各组分进行定性,分步配制液体和气体标准样品,通过分析和计算获得各物质相对于甲醇的气体体积校正因子,然后采用校正面积归一化法计算产物中的气体体积分数。经过标准气体样品的检测验证,所建立的定量分析方法可靠,最低含量物质的相对误差<7%,标准偏差在允许范围之内。

The products of oxidative carbonylation of methanol to dimethyl carbonate were analyzed on-line by gas chromatography equipped with three valves and four columns.The products were quantitated by comparison of stranded substance.The standard samples were prepared using multi-step method and the relative volume calibration factors were gained with respect to methanol,then the composition of gas products were calculated by the method of calibration area normalization.The test with standard gas show that the relative error was under 7%,the standard deviation was in the range of allowance.