体积排除色谱技术在高分子表征中的应用

刘巍; 刘勇刚; 姬相玲

doi:10.11777/j.issn1000-3304.2020.20253

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体积排除色谱技术在高分子表征中的应用

综述 (高分子表征技术专题) | 更新时间：2023-05-22

- 体积排除色谱技术在高分子表征中的应用
- Applications of Size Exclusion Chromatography in Polymer Characterization
- 高分子学报 2021年52卷第9期页码：1221-1244
- 作者机构：
  
  中国科学院长春应用化学研究所高分子物理与化学国家重点实验室长春 130022
- 作者简介：
  
  [ "刘勇刚，男，1977年生. 1998年于武汉大学获得学士学位；2004年于中国科学院长春应用化学研究所获得博士学位；之后分别在德国高分子研究所、以色列魏茨曼科学研究所、德国马普胶体与界面研究所从事博士后研究；2011年9月至今任中国科学院长春应用化学研究所副研究员，2013~2017年任中国科学院-德国马普学会“生物膜物理”伙伴小组组长. 主要研究方向为高分子溶液和生物膜物理." ]
  [ "姬相玲，女，1967年生. 1985~1995年于吉林大学高分子化学与物理专业获得学士、硕士、博士学位；1995~1997年在中国科学院长春应用化学研究所高分子物理与化学重点实验室从事博士后研究；1997~2001年中国科学院长春应用化学研究所副研究员，并于1999年赴德国美因茨大学进行合作研究. 2001年至今，中国科学院长春应用化学研究所研究员、博士生导师，2001~2003年于美国杜兰大学化工系从事博士后研究. 主要从事高分子溶液、聚烯烃链结构、多孔高分子材料等方面的研究." ]
- 基金信息：
  
  国家重点研发计划“政府间国际科技创新合作”重点专项(2018YFE0121400);国家自然科学基金(基金号 21774125)
- DOI：10.11777/j.issn1000-3304.2020.20253
  中图分类号：
- 纸质出版日期：2021-09-20，
  
  网络出版日期：2021-04-07，
  
  收稿日期：2020-11-25，
  
  修回日期：2020-12-22，
扫描看全文
刘巍,刘勇刚,姬相玲.体积排除色谱技术在高分子表征中的应用[J].高分子学报,2021,52(09):1221-1244.

Liu Wei,Liu Yong-gang,Ji Xiang-ling.Applications of Size Exclusion Chromatography in Polymer Characterization[J].ACTA POLYMERICA SINICA,2021,52(09):1221-1244.
刘巍,刘勇刚,姬相玲.体积排除色谱技术在高分子表征中的应用[J].高分子学报,2021,52(09):1221-1244. DOI： 10.11777/j.issn1000-3304.2020.20253.

Liu Wei,Liu Yong-gang,Ji Xiang-ling.Applications of Size Exclusion Chromatography in Polymer Characterization[J].ACTA POLYMERICA SINICA,2021,52(09):1221-1244. DOI： 10.11777/j.issn1000-3304.2020.20253.

摘要

体积排除色谱(SEC)也称为凝胶渗透色谱(GPC)，是利用多孔填料色谱柱将溶液中的高分子按照流体力学体积大小进行分离的一种液相色谱技术，主要用于测定各种天然和合成高分子的平均分子量及分子量分布. 多检测SEC技术可同时获得经色谱柱分离后高分子各级分的含量、分子量、均方根回转半径、流体力学半径、特性黏数等参数，进而推断高分子在溶液中的形态和链构象. 本文首先介绍了SEC分离的基本原理，即由熵驱动的高分子在多孔填料内外分配达到平衡的体积排除机理，接着总结了SEC的一些实验方法和技巧，并详细阐述了SEC在高分子的分子量及其分布测定、定量分析、链构象与刚柔性、支化结构表征、链构象转变等方面的应用，最后展望了SEC的发展趋势.

Abstract

Size exclusion chromatography (SEC)

which is also called gel permeation chromatography (GPC)

is a liquid chromatography that sorts molecules according to their hydrodynamic volume in solution by using columns packed with porous particles. It is the most frequently used technique to characterize the molecular weight and its distribution of naturally occurring and synthetic macromolecules. Multi-detector SEC combining differential refractive index

ultraviolet/visible

viscosity and multi-angle laser light scattering detectors is a powerful tool to study the shape and conformation of polymer chains in solution. Here we summarize the separation mechanism of SEC and show that the retention of polymer in SEC is an equilibrium

entropy-controlled and size-exclusion process. In order to achieve a pure SEC separation according to the size of polymer chains

enthalpy interaction between polymer chains and the packing particles should be prevented. Then we introduce the know-how to perform successful SEC experiments with a focus on the choice of eluent

column and detector

as well as sample preparation

optimization of experimental conditions and data analysis. Especially

the eluent composition should be properly optimized according to the analysed polymer sample and the column overloading should be avoided

before accurate results can be obtained by SEC. Finally

we show some examples of the recent applications of SEC in polymer characterization such as molecular weight and its distribution of polymers

composition of multi-component polymer mixtures

conformation and flexibility of polymer chains

and characterization of branched polymers. More dramatically

delayed elution of high molar mass polymers was observed in SEC at high flow rates

which is not due to polymer degradation. This abnormal elution behaviour results from a chromatographic mode transition from SEC to slalom chromatography

which originates from the coil-stretch transition of polymer chains in elongational flow through the SEC columns. It is shown that SEC can provide abundant structure parameters and their distributions of polymer chains in solution

and plays a pivotal role in the analysis of natural and synthetic macromolecules. This review aims to provide a theoretical and experimental guidance for SEC beginners

hoping to inspire more applications of SEC in the field of polymer science.

关键词

体积排除色谱高分子表征分子量及其分布构象

Keywords

Size exclusion chromatographyPolymer characterizationMolecular weight and distributionConformation

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