气相色谱法测定聚异丁烯丁二酸酐中游离酸酐  

Determination of free anhydride in polyisobutylene succinic anhydride by gas chromatography

作　　者：牛静静 王世平 杜亚珍 NIU Jingjing;WANG Shiping;DU Yazhen(Xinxiang Ruifeng New Material Co.,Ltd.,Xinxiang 453000,China)

机构地区：[1]新乡市瑞丰新材料股份有限公司,河南新乡453000

出　　处：《化学分析计量》2024年第3期65-69,87,共6页Chemical Analysis And Meterage

摘　　要：建立气相色谱法测定聚异丁烯丁二酸酐中马来酸酐含量的方法。样品用有机溶剂萃取后进色谱柱分离。色谱柱采用HP-FFAP极性毛细管柱(30 m×0.32 mm,0.25μm),载气为高纯氮气,分流比为1∶40,进样口温度为240℃,采用程序升温方式,初始温度为50℃,以10℃/min的速率升温至230℃,保持10 min,氢火焰离子化检测器温度为260℃。马来酸酐的质量分数在0~0.40%范围内与色谱峰面积线性良好,相关系数大于0.999。样品加标回收率为96.72%~99.35%,测定结果的相对标准偏差为1.172%~1.949%(n=6)。该方法操作简便、快捷、准确度高,可以满足实际生产需求。A gas chromatography method was established for determining the content of maleic anhydride in polyisobutylene succinic anhydride.The sample was extracted with organic solvents and separated by a chromatographic column.The chromatographic column was an HP-FFAP polar capillary column(30 m×0.32 mm,0.25μm).The carrier gas was high purity nitrogen with a split ratio of 1/40,the injection port temperature was 240℃,the column was heated by programmed heating,the initial temperature was 50℃,then raised at a rate of 10℃/min to 230℃,and maintained for 10 minutes.The temperature of the hydrogen flame ionization(FID)detector was 260℃.The mass fraction of maleic anhydride showed a good linear relationship with the chromatographic peak area in the range of 0-0.40%with the correlation coefficient of 0.999.The sample spiking recovery was 96.72%-99.35%,and the relative standard deviation was 1.172%-1.949%(n=6).This method has the characteristics of simple,fast,and high accuracy,and can meet practical production needs.

关 键 词：聚异丁烯丁二酸酐 马来酸酐 气相色谱法 无灰分散剂 

分 类 号：O657.7[理学—分析化学]