色谱法测定异戊烯中的微量含氧化合物-学兔兔 www.xuetutu.com.pdfVIP

学兔兔 石 油 化 工 · 1170· PETR0CHEMICAL TECHNOLOGY 2013年第42卷第10期 色谱法测定异戊烯中的微量含氧化合物 李继文，顾一丹，王 川 (中围石化 上海石油化工研究院，上海 201208) [摘要]采用GC—MS联用仪对高纯度异戊烯产品中的微量含氧化合物进行了定性分析，采用CP．Lowox毛细管色谱柱( O．53 mm×10 m)建立了异戊烯产品中微量含氧化合物的GC分析方法，对Gc分析条件进行了选择和优化，并对实际试样进行了测 定。实验结果表明，在优化的GC分析条件下，异戊烯产品中可能存在的二甲醚、甲醇、甲基叔戊基醚、叔戊醇等微量含氧化 合物分离良好。定量分析结果表明，标样的加标回收率为94．00％～108．49％，相对标准偏差均小于等于3．51％，回收率和精密 度良好；采用溶剂外标法定量，甲醇、甲基叔戊基醚、叔戊醇等组分的检测限均低于5 mg／kg。该分析方法可满足异戊烯产品 中微量含氧化合物的质量监控和实际生产过程中快速分析的需要。 [关键词]异戊烯；含氧化合物；气相色谱法；CP—Lowox毛细管色谱柱 [文章编号]1000—8144(2013)10—117O一04 [中图分类号]TQ221．214 [文献标志码]A Determination of Trace Oxygen—Compounds in Isoamylene by Gas Chromatography LiJiwen，Gu Yidan，WangChuan (SINOPEC Shanghai Research Institute ofPetrochemical Technology，Shanghai 201208，China) l Abstract J Trace oxygen-compound impurities in high purity isoamylene were separated and quanlitatively analyzed by means of GC—MS，and a new method for the determination of the trace oxygen—compounds was established by means of GC with a CP—Lowox capillary column( 0．53 mm×1 0 m1．The analytic conditions were optimized and actual samples were determined．The results showed that the oxygen—compounds existed in the isoamylene，namely dimethyl ether，methaffol， tertiary amyl methyl ether(TAME)，tert—pentanol etc．，could be separated well under the optimal chromatographic conditions．The quantitative analysis results obtained by the new method indicated that the recoveries were in the range of 94．00％一108．49％ and all the relative standard deviations were within 3．5 1％．The minimum detection cOncentrati0ns Of methano1．TAME and tert—pe