Striegel André M
Solutia Inc., 730 Worcester Street, Springfield, MA 01151, USA.
J Chromatogr A. 2003 May 9;996(1-2):45-51. doi: 10.1016/s0021-9673(03)00536-3.
Gradient polymer elution chromatography (GPEC) is rapidly becoming the analytical method of choice for determining the chemical composition distribution (CCD) of synthetic polymers. GPEC can be performed in traditional (strict precipitation-redissolution mechanism) or interactive (normal- and reversed-phase) modes, and results may be qualitative, semi-quantitative, or fully quantitative. Quantitative approaches have thus far relied on colligative or end group techniques for determining the values of standards used in constructing the GPEC calibration curve. While the values obtained from said methods are number-averages, they are assigned to the peak apexes of the standards (i.e. assigned as peak averages). This creates a determinate error in the quantitation, referred to herein as "moment bias". In this paper we determine moment bias for a series of styrene-acrylonitrile (SAN) copolymers, where the distribution and averages of the AN% have been measured using normal-phase (NP) GPEC. We also correct for the effect via statistical treatment of the chromatographic data.
梯度聚合物洗脱色谱法（GPEC）正迅速成为测定合成聚合物化学组成分布（CCD）的首选分析方法。GPEC 可以采用传统模式（严格的沉淀 - 再溶解机制）或交互式模式（正相和反相）进行，结果可以是定性、半定量或完全定量的。迄今为止，定量方法依赖于依数性或端基技术来确定构建 GPEC 校准曲线所用标准品的值。虽然从上述方法获得的值是数均分子量，但它们被指定为标准品的峰顶点值（即指定为峰平均值）。这在定量过程中产生了一个确定的误差，本文中称为“矩偏差”。在本文中，我们测定了一系列苯乙烯 - 丙烯腈（SAN）共聚物的矩偏差，其中使用正相（NP）GPEC 测量了 AN% 的分布和平均值。我们还通过对色谱数据进行统计处理来校正这种影响。
