顶空气相色谱-质谱法测定聚乙烯醇中的乙酸甲酯、甲醇和乙酸含量  

Determination of methyl acetate,methanol,acetic acid in polyvinyl alcoho1 by headspace gas chromatography-mass spectrometry

作　　者：许竞早[1] 彭振磊[1] 王川[1] 张育红[1] 白瑜[1] 

机构地区：[1]中国石化上海石油化工研究院,上海201208

出　　处：《分析仪器》2017年第2期43-49,共7页Analytical Instrumentation

摘　　要：采用顶空气相色谱-质谱法(HS/GC-MS)测定聚乙烯醇中乙酸甲酯、甲醇和乙酸等3种挥发性有机组分的残留量。采用INNOWAX毛细管柱(60m×0.25mm×0.5μm)进行分离,GC/MS定性,外标法定量。被测物乙酸甲酯、甲醇和乙酸等组分在本实验条件下均能得到很好分离,乙酸甲酯、甲醇和乙酸的校正曲线相关系数为0.9928~0.9985;样品加标回收率为89.88%~94.83%,相对标准偏差为3.83%~5.79%。本方法无需样品前处理,操作简便,测定结果准确可靠,适用于聚乙烯醇及类似高分子材料中残留有机组分的检测。The chromatographic column was INNOWAX （60m × 0.25mm, 0.5 μm） capillary column. The qualitative and quantitative analysises were performed by GC/MS. The external calibration was used for the quantification. The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship（r： 09928 -0. 9985） with good precision and accuracy. The addition standard recovery was in the range of 89.23%--94.24% and the relative standard deviations （RSDs） were between 4.09% and 6.12%. The established method is accurate and reliable. It can be used for the determination of residual solvents in polyvinyl alcohol and other polymer materials.

关 键 词：聚乙烯醇 挥发性有机组分 乙酸甲酯 甲醇 乙酸 顶空气相色谱-质谱法 

分 类 号：TQ317.2[化学工程—高聚物工业] O657.63[理学—分析化学]