色谱

色谱 ›› 2017, Vol. 35 ›› Issue (5): 538-543.DOI: 10.3724/SP.J.1123.2016.11022

• 研究论文 • 上一篇    下一篇

在线固相萃取-离子色谱法测定4种芳环磺酸盐中的硫酸根离子

陈爱连, 方琳美, 吕海霞, 施超欧   

  1. 华东理工大学化学与分子工程学院, 分析测试中心, 上海 200237
  • 收稿日期:2016-11-23 出版日期:2017-05-08 发布日期:2013-08-28
  • 通讯作者: 张吉苹,E-mail:shico@ecust.edu.cn.

Determination of sulfate ion in four aromatic sulfonates by ion chromatography coupled with on-line solid phase extraction

CHEN Ailian, FANG Linmei, LÜ Haixia, SHI Chaoou   

  1. Analysis and Testing Center, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China
  • Received:2016-11-23 Online:2017-05-08 Published:2013-08-28

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70

被引次数

2

摘要：

建立一种在线固相萃取-离子色谱测定4种芳环磺酸盐中硫酸根离子含量的新方法。将自装填的多孔石墨化碳固相萃取柱应用于离子色谱系统，对样品进行在线前处理。样品经过多孔石墨化碳固相萃取柱基体消除后进入收集环，通过阀切换方式使待测硫酸根离子转入阴离子分析柱和检测系统。固相萃取流路用1.5 mmol/L碳酸钠以0.8 mL/min的流速对基体在线富集，进样量为20μL，分析柱为SH-AC-3（250 mm×4.0 mm）+SH-AG-3（50 mm×4.0 mm）色谱柱，柱温为35℃，在6 mmol/L碳酸钠-4 mmol/L碳酸氢钠条件下等度洗脱，流速为0.8 mL/min。结果表明：硫酸根离子在0.50~20.00 mg/L范围内呈良好的线性关系，线性相关系数为0.9983，保留时间、峰高和峰面积的相对标准偏差均在0.28%~2.86%之间，方法检出限为0.0106 mg/L，回收率为91.01%~109.3%，具有良好的线性关系和重复性。整个在线分析过程在25 min之内完成。该方法进样量少、快速、高效。

关键词: 多孔石墨化碳, 芳环磺酸盐, 离子色谱, 硫酸根离子, 在线固相萃取, 自装填技术

Abstract:

A new ion chromatography method coupled with on-line solid phase extraction was developed for the determination of sulfate ion in four aromatic sulfonates. A self packed porous graphitized carbon solid phase extraction (PGC-SPE) column was used for on-line sample pre-treatment and a valve switching-large volume injection mode was used for sample injection in the system. After processed by PGC-SPE column, the inorganic ions contained in samples got into a loop and then were flushed into the detection system. The eluent of SPE for on-line matrix enrichment was 1.5 mmol/L sodium carbonate at a flow rate of 0.8 mL/min. The injection volume was 20 μL. The analytical columns were SH-AC-3 (250 mm×4.0 mm)+SH-AG-3 (50 mm×4.0 mm). The column temperature was set at 35℃. The elution was performed by 6 mmol/L sodium carbonate-4 mmol/L sodium bicarbonate at a flow rate of 0.8 mL/min. The results showed that the sulfate ion in the range of 0.50-20.00 mg/L had a good linear relationship and the correlation coefficient was 0.9983. The relative standard deviations (RSDs) of the retention time, peak height and peak area were 0.28%-2.86%. The limit of detection was 0.0106 mg/L. The recoveries were 91.01%-109.3%. The entire online analysis process was completed within 25 min with small injection volume, short analysis time and high efficiency. This method possesses good linearity and repeatability.

Key words: aromatic sulfonates, ion chromatography (IC), on-line solid phase extraction (on-line SPE), porous graphitized carbon (PGC), self-packing technology, sulfate ion

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