离心场场流分离联用静态光散射测量聚合物分子质量的方法
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摘要
以Na Cl溶液为流动相,采用离心场场流分离仪对样品进行分级,结合静态光散射仪、示差折光检测器测定亲水性弱聚电解质聚丙烯酸的数均分子质量及重均分子质量。通过考察流动相流速、离心场的离心转速等影响离心分离的因素,确定仪器可准确测量的条件。结果表明,当流动相流速为0. 7 m L/min、离心场转速为3 500 r/min时,该装置可准确测定聚丙烯酸的平均分子质量。
Na Cl solution is used as the mobile phase and the sample is classified by a centrifugal field flow separator.Through combining with static light scattering instrument and refractive index detector,the number-average molecular weight and weight-average molecular weight of hydrophilic weak polyelectrolyte polyacrylic acid are determined.The conditions that can allow instrument to measure accurately are determined by studying the factors that affect the centrifugal separation,such as flow rate of the mobile phase and the centrifugal speed of the centrifugal field.The results show that this device can determine accurately the average molecular weight of polyacrylic acid when the mobile phase flow rate is 0. 7 m L·min-1 and the centrifugal field speed is 3 500 r·min-1.
Na Cl solution is used as the mobile phase and the sample is classified by a centrifugal field flow separator.Through combining with static light scattering instrument and refractive index detector,the number-average molecular weight and weight-average molecular weight of hydrophilic weak polyelectrolyte polyacrylic acid are determined.The conditions that can allow instrument to measure accurately are determined by studying the factors that affect the centrifugal separation,such as flow rate of the mobile phase and the centrifugal speed of the centrifugal field.The results show that this device can determine accurately the average molecular weight of polyacrylic acid when the mobile phase flow rate is 0. 7 m L·min-1 and the centrifugal field speed is 3 500 r·min-1.
引文
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[15]叶祥喜,宋燕西,陈旭涛,等.高效液相色谱手性流动相添加剂法拆分佐匹克隆对映体[J].分析测试学报,2014,33(4):471-474.
[2]潘雨生.关于气相渗透法仪器常数对分子量依赖性的讨论[J].高分子学报,1981,1(2):158-160.
[3]Lozano D C P,Orrego-Ruiz J A,Barrow M P,et al.Analysis of the molecular weight distribution of vacuum residues and their molecular distillation fractions by laser desorption ionization mass spectrometry[J].Fuel,2016,171:247-252.
[4]Wang Z,Chi L.Recent advances in mass spectrometry analysis of low molecular weight heparins[J].Chinese Chemical Letters,2018,29(1):11-18.
[5]刘洪兵,刘红颖.超高分子量聚合物特性粘数测定方法探讨[J].大庆石油地质与开发,2001,20(2):104-105.
[6]丁勇,吴红枚,王孟,等.聚间苯二甲酰对苯二胺(PPIA)数均分子量的测定[J].山东化工,2016,45(11):74-77.
[7]王明君,姚善泾.小角激光光散射法测定纤维素硫酸钠的分子量[J].过程工程学报,2009,9(6):1159-1163.
[8]冯茹森,郭拥军,张新民,等.疏水缔合聚合物分子量分布曲线的测定[J].高分子学报,2016(5):621-627.
[9]Kim R Williams,Karin D Caldwell.Field-flow fractionation[J].Analytical and Bioanalytical Chemistry,2014,406:1577-1578.
[10]Greyling G,Pasch H.Fractionation of poly(methacrylic acid)and poly(vinyl pyridine)in aqueous and organic mobile phases by multidetector thermal field-flow fractionation[J].Journal of Chromatography A,2017,1512:115-123.
[11]Roessner D,Kulicke W M.On-line coupling of flow field-flow fractionation and multi-angle laser light scattering[J].Journal of Chromatography A,1994,687(2):249-258.
[12]Wagner M,Pietsch C,Tauhardt L,et al.Characterization of cationic polymers by asymmetric flow field-flow fractionation and multi-angle light scattering-A comparison with traditional techniques[J].Journal of Chromatography A,2014,1325(2):195-203.
[13]Ugo Till,Mireille Gaucher-Delmas,et al. Asymmetrical flow fieldflow fractionation with multi-angle light scattering and quasi-elastic light scattering for characterization of polymersomes:Comparison with classical techniques[J]. Analytical and Bioanalytical Chemistry,2014,406:7841-7853.
[14]赵希贤,尤立华,杨秉呼,等.土茯苓含量测定分离度和理论板数的调整[J].首都医药,2013,20(24):69-70.
[15]叶祥喜,宋燕西,陈旭涛,等.高效液相色谱手性流动相添加剂法拆分佐匹克隆对映体[J].分析测试学报,2014,33(4):471-474.