色谱

色谱 ›› 2016, Vol. 34 ›› Issue (10): 976-981.DOI: 10.3724/SP.J.1123.2016.06047

• 特别策划:离子态化合物色谱分析专栏 • 上一篇    下一篇

离子色谱法检测高纯硅微粉中痕量铁和氧化铁杂质

罗进1,3, 郑洪国2, 李仁勇2, 赵海能1, 李超1, 赵炯1,4, 李春林1,4   

  1. 1. 四川省分析测试服务中心, 成都 610023;
    2. 赛默飞世尔科技(中国)有限公司, 四川 成都 610023;
    3. 四川大学分析测试中心, 四川 成都 610023;
    4. 四川赛纳斯分析检测有限公司, 四川 成都 610023
  • 收稿日期:2016-06-28 出版日期:2016-10-08 发布日期:2013-04-03
  • 通讯作者: 罗进
  • 基金资助:

    四川省科技支撑计划项目（2015FZ0097）.

Determination of trace impurities of iron and ferric oxide in high purity microsilica by ion chromatography

LUO Jin1,3, ZHENG Hongguo2, LI Renyong2, ZHAO Haineng1, LI Chao1, ZHAO Jiong1,4, LI Chunlin1,4   

  1. 1. Sichuan Analysis and Testing Center, Chengdu 610023, China;
    2. Thermo Fisher Scientific Inc., Chengdu 610023, China;
    3. Analytical Center of Sichuan University, Chengdu 610023, China;
    4. Sichuan Sainasi Analytical and Testing Co., Ltd., Chengdu 610023, China
  • Received:2016-06-28 Online:2016-10-08 Published:2013-04-03
  • Supported by:

    Sichuan Science and Technology Support Program (No. 2015FZ0097).

PDF

156

被引次数

2

摘要：

建立了柱后衍生-紫外检测-离子色谱法同时测定高纯硅微粉中痕量铁和氧化铁杂质含量的方法。方法选用具有阴阳离子交换基团的高选择性Thermo Scientific DionexTM IonPacTM CS5A色谱柱，选择与铁形成单一络合形态、中等络合能力的2，6-吡啶二羧酸（PDCA）为淋洗液，在线柱后添加普适性的4-2-吡啶偶氮苯二酚（PAR）金属显色剂，于530 nm波长下准确完成了二价和三价铁离子的分离测定。结果表明，本方法对二价铁离子和三价铁离子的检出限分别为0.013 mg/kg和0.006 mg/kg，线性相关系数r2均大于0.999，实际样品中二价铁和三价铁的加标回收率分别为79%~90%和92%~105%，具有较高的灵敏度、准确度和选择性。该方法可以准确测定高纯硅微粉中痕量二价铁和三价铁的含量，以此结果反馈高纯硅微粉产品中铁杂质含量的不同来源，为其生产工艺的持续优化和改进提供重要的参考数据。

关键词: 硅微粉, 离子色谱法, 铁, 氧化铁, 柱后衍生

Abstract:

A method for detecting trace impurities of iron and ferric oxide in high purity microsilica was established by ion chromatography with post column derivatization plus UV detection. The separation of ferric and ferrous was achieved on Thermo Scientific DionexTM IonPacTM CS5A column containing anion and cation exchange functional groups with 2,6-pyridinedicarboxylic acid (PDCA) solution elution. The target compounds were derivatized with 4-(2-pyridylazo)resorcinol (PAR) and detected at 530 nm. The limits of detection for ferrous and ferric were 0.013 mg/kg and 0.006 mg/kg respectively. Both of the linear correlation coefficients for ferrous and ferric were better than 0.999. The recoveries of ferrous and ferric were 79%-90% and 92%-105% respectively. The method provides high sensitivity, high accuracy and high selectivity for the detection of ferrous and ferric in microsilica, which would be used for monitoring the different sources of iron in microsilica industry.

Key words: ferric oxide, ferrous, ion chromatography (IC), microsilica, post column derivatization

中图分类号: