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通过选择性衍生化后进行尺寸排阻色谱法对聚合羧酸官能团进行异质性分析。

Heterogeneity analysis of polymeric carboxylic acid functionality by selective derivatization followed by size exclusion chromatography.

作者信息

Brooijmans T, Okhuijsen R A, Oerlemans G M M, Pirok B W J, Schoenmakers P J, Peters R A H

机构信息

DSM Coating Resins, Analytical Technology Centre, Waalwijk, the Netherlands.

DSM Coating Resins, Analytical Technology Centre, Waalwijk, the Netherlands.

出版信息

Anal Chim Acta. 2019 Sep 23;1072:87-94. doi: 10.1016/j.aca.2019.04.051. Epub 2019 Apr 25.

DOI:10.1016/j.aca.2019.04.051
PMID:31146869
Abstract

Waterborne polymers are increasingly applied in our society, replacing traditional solvent-borne coatings and thus reducing environmental impact of coatings. The majority of waterborne dispersions are stabilized by the incorporation of neutralizable carboxylic acid functionality. The characterization of synthetic waterborne polymer systems can be performed by a wide variety of chromatographic and spectroscopic techniques. However, none of these approaches is able to determine the acid functionality distribution over the molecular-weight distribution directly. In this research, an innovative approach is developed which enables this analysis. The approach is based on the specific and complete derivatization of carboxylic acid functionality with phenacylbromide. Size exclusion chromatography (SEC) analysis of the derivatized polymers is performed followed by ultraviolet- (UV) and refractive index (RI) detection, enabling the quantitative determination of the acid content per molecular weight fraction. The applicability of the developed protocol is shown for various polymer systems.

摘要

水性聚合物在我们的社会中应用越来越广泛,取代了传统的溶剂型涂料,从而降低了涂料对环境的影响。大多数水性分散体通过引入可中和的羧酸官能团来实现稳定化。合成水性聚合物体系的表征可以通过多种色谱和光谱技术来进行。然而,这些方法都无法直接确定酸官能团在分子量分布上的分布情况。在本研究中,开发了一种创新方法来实现这种分析。该方法基于用苯甲酰溴对羧酸官能团进行特异性和完全衍生化。对衍生化后的聚合物进行尺寸排阻色谱(SEC)分析,随后进行紫外(UV)和折射率(RI)检测,从而能够定量测定每个分子量级分的酸含量。所开发的方案对各种聚合物体系的适用性也得到了展示。

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