色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 88-91.DOI: 10.3724/SP.J.1123.2012.08001

• 技术与应用 • 上一篇    

阀切换-离子色谱法测定分析纯硫酸钠中痕量氯离子

张婷婷1*, 王娜妮2, 叶明立1, 胡忠阳1, 潘广文1   

  1. 1. 赛默飞世尔科技有限公司上海实验室, 上海 201203; 2. 浙江大学化学系, 浙江 杭州 310028
  • 收稿日期:2012-08-01 修回日期:2012-10-17 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: 张婷婷
  • 基金资助:

    浙江省省级公益性技术应用研究计划项目(2012C37038).

Determination of trace chloride in sodium sulfate of analytical reagent-grade by valve-switching ion chromatography

ZHANG Tingting1*, WANG Nani2, YE Mingli1, HU Zhongyang1, PAN Guangwen1   

  1. 1. Shanghai Lab, Thermo Fisher Scientific Inc., Shanghai 201203, China; 2. Department of Chemistry, Zhejiang University, Hangzhou 310028, China
  • Received:2012-08-01 Revised:2012-10-17 Online:2013-01-28 Published:2013-01-21

PDF

520

被引次数

11

摘要： 建立了阀切换-离子色谱法测定分析纯硫酸钠固体中痕量氯离子含量的方法。ICS-2100离子色谱系统,配置十通阀,用IonPac AS18色谱柱将硫酸钠固体样品中的氯离子和硫酸根离子预分离后,以IonPac TAC-ULP1为富集柱,将氯离子富集后在相同的IonPac AS18色谱柱上进行定量分析。同时以淋洗液发生器产生的不同浓度的KOH作为淋洗液,以抑制型电导检测器测定氯离子的含量。结果表明,阀切换-离子色谱法测定分析纯硫酸钠固体中的痕量氯离子,检出限为10 μg/L,线性相关系数(r2)大于0.999,实际样品的加标回收率为98.0%～103.0%,具有分离度和灵敏度高,选择性好,操作简单等特点。该方法能够准确测定硫酸钠固体中痕量氯离子的含量,适用于高纯化学试剂中痕量氯离子的分离测定。

关键词: 阀切换, 分析纯硫酸钠, 离子色谱, 氯离子

Abstract: A valve-switching ion chromatography system was developed for the determination of trace chloride in sodium sulfate using a single pump, a suppressor, two valves and three columns. Using this technique, the trace chloride was eluted from the concentrator column (IonPac TAC-ULP1, 23 mm×5 mm) to the analytical column (IonPac AS18, 250 mm×4 mm), and the sulfate flowed to the waste. Under the optimized separation conditions, the method showed good linearity (r2＞0.999) in the range of 0.03-1 mg/L and the average recoveries of chloride were 98.0%-103.0% with the relative standard deviation less than 2%. The limit of detection was 0.01 mg/L (S/N=3). The results demonstrated that this system has the advantages of high sensitivity, facile automation and simple sample pretreatment, which might be a promising approach for the determination of trace chloride in high-purity reagents.

Key words: chloride, sodium sulfate of analytical reagent-grade, valve-switching, ion chromatography (IC)