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Sulfonic Acid Group Determination in Lignosulfonates by Headspace Gas Chromatography
ACS Sustainable Chemistry & Engineering ( IF 7.1 ) Pub Date : 2018-04-16 00:00:00 , DOI: 10.1021/acssuschemeng.8b00011 Philipp Korntner 1 , Andreas Schedl 1 , Ivan Sumerskii 1 , Thomas Zweckmair 1 , Arnulf Kai Mahler 2 , Thomas Rosenau 1 , Antje Potthast 1
ACS Sustainable Chemistry & Engineering ( IF 7.1 ) Pub Date : 2018-04-16 00:00:00 , DOI: 10.1021/acssuschemeng.8b00011 Philipp Korntner 1 , Andreas Schedl 1 , Ivan Sumerskii 1 , Thomas Zweckmair 1 , Arnulf Kai Mahler 2 , Thomas Rosenau 1 , Antje Potthast 1
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A method for the determination of the sulfonic acid content in lignosulfonates via sulfur dioxide quantification upon treatment with H3PO4 by headspace gas chromatography is presented and compared to two already established alternatives, conductometric titration and elemental analysis. Several lignosulfonates, purified from various industrial sources, were examined by all three methods. Limitations and possible interference by other functional groups, such as carboxylic acids, are discussed, and suitable solutions are presented. Results of the novel approach are comparable to those of the established techniques in terms of accuracy and precision. The limit of detection (LOD) is 0.88 μmol of SO3H and the corresponding limit of quantification (LOQ) is 3.78 μmol of SO3H. At the same time, this method outperforms conductometric titration in terms of a higher sample throughput and a much smaller sample amount needed for analysis. Treatment of the sample with highly concentrated phosphoric acid and simple heating is straightforward enough to render the method a valuable tool in lignosulfonate analysis of industrial problem sets, such as screenings or optimization of process parameters, without compromising analytical accuracy.
中文翻译：
顶空气相色谱法测定木质素磺酸盐中的磺酸基
提出了一种通过顶空气相色谱法在用H 3 PO 4处理后通过二氧化硫定量测定木质素磺酸盐中磺酸含量的方法，并将其与电导滴定和元素分析这两个已经建立的替代方法进行了比较。通过所有三种方法检查了从各种工业来源纯化得到的几种木质素磺酸盐。讨论了其他官能团（例如羧酸）的局限性和可能的干扰，并提出了合适的解决方案。就准确性和精确度而言，新方法的结果可与现有技术的结果相提并论。SO 3的检出限（LOD）为0.88μmolH和定量的相应的限制（LOQ）为3.78微摩尔的SO 3 H.同时，此方法优于电导滴定在更高的采样的吞吐量和分析所需小得多的样品量而言。用高浓度磷酸处理样品并简单加热就足够简单，这使得该方法成为工业问题集木质素磺酸盐分析的有价值的工具，例如筛选或优化工艺参数，而不会影响分析精度。
更新日期：2018-04-16
中文翻译：
顶空气相色谱法测定木质素磺酸盐中的磺酸基
提出了一种通过顶空气相色谱法在用H 3 PO 4处理后通过二氧化硫定量测定木质素磺酸盐中磺酸含量的方法，并将其与电导滴定和元素分析这两个已经建立的替代方法进行了比较。通过所有三种方法检查了从各种工业来源纯化得到的几种木质素磺酸盐。讨论了其他官能团（例如羧酸）的局限性和可能的干扰，并提出了合适的解决方案。就准确性和精确度而言，新方法的结果可与现有技术的结果相提并论。SO 3的检出限（LOD）为0.88μmolH和定量的相应的限制（LOQ）为3.78微摩尔的SO 3 H.同时，此方法优于电导滴定在更高的采样的吞吐量和分析所需小得多的样品量而言。用高浓度磷酸处理样品并简单加热就足够简单，这使得该方法成为工业问题集木质素磺酸盐分析的有价值的工具，例如筛选或优化工艺参数，而不会影响分析精度。
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