Striegel André M
Solutia Inc., Springfield, MA 01151, USA.
J Chromatogr A. 2002 Sep 20;971(1-2):151-8. doi: 10.1016/s0021-9673(02)00960-3.
The vinyl alcohol (VOH) functionality in poly(vinyl butyral) is known to be responsible for a number of important end-use properties, such as controlling adhesion to surfaces, influencing cross-linking behavior, etc. In order to determine the distribution of the VOH percentage in PVB, with the associated averages and polydispersity, we have developed a normal-phase gradient polymer elution chromatography (NP-GPEC) method which relies on both precipitation-redissolution as well as on sorptive interactions between the polymer and the column packing. The method is shown to operate in the linear region of detector response with respect to key operational parameters and is demonstrated to be independent of chemical composition distribution, molar mass, or polydispersity in either molar mass or VOH content. Several examples are given, including where NP-GPEC readily allows visualization of differences between samples that appear identical when analyzed by standard methods.
众所周知，聚乙烯醇缩丁醛中的乙烯醇（VOH）官能团决定了许多重要的最终使用性能，例如控制对表面的附着力、影响交联行为等。为了确定聚乙烯醇缩丁醛（PVB）中VOH百分比的分布以及相关的平均值和多分散性，我们开发了一种正相梯度聚合物洗脱色谱法（NP-GPEC），该方法依赖于沉淀-再溶解以及聚合物与柱填料之间的吸附相互作用。结果表明，该方法在检测器响应的线性区域内针对关键操作参数运行，并且证明与化学组成分布、摩尔质量或摩尔质量或VOH含量的多分散性无关。给出了几个例子，包括NP-GPEC能够轻松显示通过标准方法分析时看似相同的样品之间的差异。
