State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou, China.
J Chromatogr A. 2012 Mar 16;1229:302-4. doi: 10.1016/j.chroma.2012.01.058. Epub 2012 Jan 25.
This paper reports on a headspace gas chromatographic method (HS-GC) for rapid determination of degree of substitution in succinic anhydride (SA) modified celluloses. The method is based on the reaction between the carboxyl groups in SA modified cellulose and bicarbonate solution in a closed headspace sample vial. The CO(2) released from the reaction was measured by HS-GC. The completion of the reaction was achieved within 25 min at 80 °C when a small sample size (<20 mg) was used. The relative standard deviation (RSD) measurement of precision was less than 4.1%, and the results were within 8.0% of those obtained with the traditional titration for determining the degree of substitution. The present method is simple, practical, automated, and suitable for use in anhydride modified cellulose research.
本文报道了一种快速测定琥珀酸酐（SA）改性纤维素取代度的顶空气相色谱法（HS-GC）。该方法基于在封闭的顶空样品瓶中，SA 改性纤维素中的羧基与碳酸氢盐溶液之间的反应。通过 HS-GC 测量反应释放的 CO₂。当使用小样品量（<20mg）时，在 80°C 下 25 分钟内即可完成反应。精密度的相对标准偏差（RSD）测量值小于 4.1%，并且与传统滴定法测定取代度的结果相差在 8.0%以内。本方法简单、实用、自动化，适用于酐改性纤维素的研究。
