色谱

色谱 ›› 2014, Vol. 32 ›› Issue (2): 204-209.DOI: 10.3724/SP.J.1123.2013.09038

• 技术与应用 • 上一篇    

离子色谱法测定合成气制烯烃产物中的C1~C6有机酸

顾一丹1,2, 李继文1, 宋卫林1,2, 张祥民2   

  1. 1. 上海石油化工研究院, 上海 201208;
    2. 复旦大学化学系, 上海 200433
  • 收稿日期:2013-09-23 修回日期:2013-11-26 出版日期:2014-02-08 发布日期:2014-01-25
  • 通讯作者: 李继文， 张祥民

Determination of C1-C6 organic acids in the products from syngas to olefins by ion chromatography

GU Yidan1,2, LI Jiwen1, SONG Weilin1,2, ZHANG Xiangmin2   

  1. 1. SINOPEC Shanghai Research Institute of Petrochemical Technology, Shanghai 201208, China;
    2. Department of Chemistry, Fudan University, Shanghai 200433, China
  • Received:2013-09-23 Revised:2013-11-26 Online:2014-02-08 Published:2014-01-25

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摘要：

采用离子色谱建立了合成气制烯烃(SGTO)水相产物和油相产物中C1~C6有机酸的测定方法。对分离条件进行了优化，使用标准样品测定了线性范围和工作曲线，考察了方法的精密度和准确度，确定了SGTO油相产物样品的碱洗条件，并对SGTO水相产物和油相产物样品进行了测定。结果表明：C1~C6有机酸的质量浓度在各自配制的质量浓度范围内呈现良好的线性关系，相关系数均大于0.99。标准溶液的回收率测定表明回收率在95.6%~104.3%之间，5次重复测定的相对标准偏差(RSD)在0.4%~3.6%之间，表明该方法具有良好的准确性和精密度。SGTO油相产物中的加标回收率在91.1%~96.8%之间，5次重复测定的RSD为0.7%~2.3%，准确性可以满足实际分析的需要。实际SGTO水相产物和油相产物中C1~C6有机酸的分析结果表明，SGTO水相产物中C2~C4有机酸含量较高，而SGTO油相产物中C4~C6有机酸含量较高。本研究对SGTO反应研究、催化剂制备、工艺优化以及设备材料的选择具有重要意义。

关键词: C1~C6有机酸, 合成气制烯烃, 离子色谱, 水相产物, 油相产物

Abstract:

A method for the determination of C1-C6 organic acids in the products from syngas to olefins (SGTO) was developed by ion chromatography, which included the optimized separation conditions, the linear ranges and the working curves determined by using standard samples, the precision and accuracy of the method and the alkaline-washing conditions of the pretreatment for the oil phase samples. The SGTO water phase and oil phase samples were analyzed according to the method. The linearity test showed that the correlation coefficients (R2) for all of the C1-C6 organic acids in the specific concentration ranges were above 0.99, which means that all the components had good linear correlations. The recoveries of standard solutions were from 95.6% to 104.3%, and the RSDs (n=5) were from 0.4% to 3.6%. The spiked recoveries in SGTO oil phase samples were from 91.1% to 96.8%, and the RSDs (n=5) were from 0.7% to 2.3%. The accuracy of the method can satisfy the requirement for the analysis of SGTO samples. The results showed that there were more C2-C4 organic acids in the water phase samples, while there were more C4-C6 organic acids in the oil phase samples. This research has great significance for the study of SGTO reaction, the improvements of catalysts and operation conditions, and is helpful for choosing the materials of the equipment.

Key words: C1~C6 organic acids, ion chromatography (IC), oil phase products, syngas to olefins(SGTO), water phase products

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