联合超高效聚合物色谱和激光光散射法的聚酯分子质量及其分布测定

纺织学报 ›› 2016, Vol. 37 ›› Issue (05): 11-16.

联合超高效聚合物色谱和激光光散射法的聚酯分子质量及其分布测定

收稿日期:2015-04-27 修回日期:2016-02-19 出版日期:2016-05-15 发布日期:2016-05-10

Determination of polyester molecular weight and its distribution by advanced polymer chromatography and laser light scattering detector

Received:2015-04-27 Revised:2016-02-19 Online:2016-05-15 Published:2016-05-10

摘要/Abstract

摘要：

将超高效聚合物色谱-多角度激光光散射仪（APC-MALLS）联用建立了一种新型测试聚对苯二甲酸乙二醇酯（PET）分子质量及其分布的方法，确定了含三氟乙酸钠的六氟异丙醇（HFIP）作为溶剂和流动相的测试体系；并通过优化样品浓度、流动相流速等测试条件获得了不同特性黏度PET样品的分子质量及其分布。结果表明，所建立的测试方法无需用标准样校正即可获得样品的绝对分子质量，比传统GPC测试方法速度提高4倍以上，重复性实验结果误差小于2%。实验测得特性粘度为0.685、0.884、1.038 dL/g的样品数均分子质量分别为22 700、32 000、41 600，分子质量分布分别为1.62、1.56、1.55。

关键词: 超高效聚合物色谱, 多角度激光光散射, 聚酯, 分子质量分布

Abstract:

Coupled advanced polymer chromatography with multi-angle laser light scattering (APC-MALLS), the novel method for measuring the molecular weight and molecular weight distribution of polyethylene terephthalate (PET) was developed successfully. In this measuring system, hexafluoroisopropanol containing sodium trifluoroacetate was chosen as solvent in which several different intrinsic viscosity of PET could be dissolved effectively and quickly at room temperature, it can also be used as an eluent. The effect of the sample concentration and flow rate were discussed. There is no need to set a calibration by the use of standard samples, and the absolute molecular weight and molecular weight distribution of PET were acquired in several minutes under the optimum condition. Comparing with the conventional GPC method, such an efficient test system can greatly shorten the testing time, simplify the test procedures and presents the excellent repeatability. The number-average molecular weight of the samples（intrinsic viscosity：0.685, 0.884, 1.038 dL/g）were 22 700, 32 000, 41 600 g/mol and the molecular weight distribution were 1.62、1.56、1.55.

Key words: advanced polymer chromatography, multi-angle laser light scattering, poly(ethylene terephthalate), Molecular weight distribution

中图分类号:

刘梅刘雄陈世昌吕汪洋李楠陈文兴. 联合超高效聚合物色谱和激光光散射法的聚酯分子质量及其分布测定[J]. 纺织学报, 2016, 37(05): 11-16.

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