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色谱法测定聚苯酯基复合材料组成的研究

Determination of POB in POB-based Composites by High Performance Liquid Chromatography

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【作者】 王建郭亚芸于素华杨晨胡效亚赵文轸

【Author】 WANG Jian1,2,GUO Ya-yun1,YU Su-hua1,YANG Chen1,HU Xiao-ya1,ZHAO Wen-zhen2(1 School of Chemistry & Chemical Engineering,Yangzhou University,Key Laboratory of Environmental Materials & Engineering of Jiangsu Province,Jiangsu Yangzhou 225002;2 School of Materials Science and Engineering,Xi’an Jiaotong University,Shaanxi Xi’an 710049,China)

【机构】 扬州大学化学化工学院江苏省环境材料与环境工程重点实验室西安交通大学材料与工程学院

【摘要】 以气相色谱法测定聚苯酯降解物CH3COOH,在分离度、色谱峰形或数据重复性方面不能满足定量测定要求。以高效液相色谱法在254 nm时测定POB降解溶液中的对羟基苯甲酸,方法的灵敏度(LOD 9.95×10-12mol/L)、重现性(RSD小于0.6%)、回收率(87.88%~107.51%)、线性相关性(线性相关系数0.99以上)都满足定量测定要求;根据聚苯酯降解液中的p-HBA测得所合成POB聚合度为27.6,测定POB基复合材料中POB的质量分数时发现,以不同配方合成的复合材料中POB的质量分数都与理论值有较大偏离,这一现象可能由合成聚苯酯时单体升华损失所致。

【Abstract】 Low resolution,asymmetric peaks or poor reproducibility were discovered while CH3COOH degraded from POB was analyzed by GC.When p-HBA in the degradation product was analyzed by High Performance Liquid Chromatography(HPLC),good linearities(Linear correlation coefficient above 0.99),high recoveries(87.88%~107.51%),excellent reproducibilities(RSD below 0.6%) as well as low LOD(9.95×10-12 mol/L) can be achieved at 254 nm.The polymerization degree of POB was determined as 27.6 by this method.The mass fraction of POB in its composites was found to be lower than the calculated values,which maybe due to the sublimation of p-ABA.

【基金】 国家自然科学基金资助项目(20675071)
  • 【文献出处】 广州化工 ,Guangzhou Chemical Industry , 编辑部邮箱 ,2011年01期
  • 【分类号】TB332
  • 【下载频次】73
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