离子色谱柱切换法测定氟化盐高纯试剂中的阴离子杂质

引用本文: 胡忠阳, 叶明立, 吴述超, 潘广文, 张婷婷, 刘绿叶. 离子色谱柱切换法测定氟化盐高纯试剂中的阴离子杂质[J]. 分析化学, 2012, 40(11): 1703-1708. doi: 10.3724/SP.J.1096.2012.20213 shu

Citation: HU Zhong-Yang, YE Ming-Li, WU Shu-Chao, PAN Guang-Wen, ZHANG Ting-Ting, LIU LÜ-Ye. Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching[J]. Chinese Journal of Analytical Chemistry, 2012, 40(11): 1703-1708. doi: 10.3724/SP.J.1096.2012.20213 shu

离子色谱柱切换法测定氟化盐高纯试剂中的阴离子杂质

胡忠阳 ^{1,
,} ,
叶明立 ^1, ,
吴述超 ^2, ,
潘广文 ^1, ,
张婷婷 ^1, ,
刘绿叶 ^1,

通讯作者: 胡忠阳

基金项目:
本文系浙江大学国家重点实验室开放基金项目(No. 2011KF07) (No. 2011KF07)

安徽省教育厅高校科研项目(No. KJ2011B211)资助 (No. KJ2011B211)

摘要: 建立了一种测定高纯氟化盐试剂中杂质阴离子的离子色谱柱切换技术分析方法。在纯水流动相下,采用IonPac ICE-AS6离子排斥柱将待测杂质Cl^-, SO₄^2-, NO₃^-及PO₄^3-从高浓度的氟化盐溶液中分离出来,分离出的待测组分富集于IonPac TAC-ULP1浓缩柱上。以4.5 mmol/L Na₂CO₃-0.8 mmol/L NaHCO₃为淋洗液,流速1.2 mL/min,经过柱切换,将待测离子从浓缩柱上洗脱下来,通过IonPac AG23 (50 mm×4 mm) 和IonPac AS23 (250 mm×4 mm)色谱柱进行分离,抑制电导检测器检测。本方法在线性范围内,Cl^-, NO₃^-, PO₄^3-和SO₄^2-的相关系数分别为0.9996, 0.9999, 0.9998和0.9997;加标回收率为92.0%-103.5%;相对标准偏差RSD (n=7)均小于3.0%;检出限(S/N=3)分别为0.2, 0.6, 3.0和0.5 mg/kg。

关键词:

English

Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching

1.
¹ Thermofisher Scientific Corporation, Shanghai 201203, China;

Corresponding author: 胡忠阳

Received Date: 02 March 2012
Fund Project:
本文系浙江大学国家重点实验室开放基金项目(No. 2011KF07)

安徽省教育厅高校科研项目(No. KJ2011B211)资助

Abstract: A method was developed for the determination of trace anions (Cl^-, NO₃^-, PO₄^3- and SO₄^2-) in high pure fluoride reagents by ion chromatography (IC) with column-switching. Ion excluding column IonPac ICE-AS6 was used in the first step to separate the trace anion analytes from the high concentrated fluoride using deionized water as the mobile phase, separated analytes were enriched in the pre-concentration column IonPac TAC-ULP1 at the same time. By using a mixture of 4.5 mmol/L Na₂CO₃-0.8 mmol/L NaHCO₃ as the eluent at a flow rate of 1.2 mL/min, the analytes were eluted from the pre-concentrated column after switching the pre-concentrated column into the analytical system. The separation of the analytes was performed with IonPac AG23 (50 mm × 4 mm) as guard column and IonPac AS23 (250 mm×4 mm) as analytical column, and the detection was performed by suppressed conductivity detector. As a result, the linear ranges of the method for Cl^-, NO₃^-, PO₄^3- and SO₄^2- were 0.02-5.0 mg/L (r=0.9996), 0.02-5.0 mg/L (r=0.9999), 0.05-10.0 mg/L (r=0.9998), 0.02-5.0 mg/L (r=0.9997) respectively. The average recoveries were 92.0%-103.5% with the relative standard deviations (RSD, n=7) less than 3.0%. The detection limits (S/N=3) were 0.2, 0.6, 3.0 and 0.5 mg/kg for Cl^-, NO₃^-, PO₄^3-and SO₄^2-, respectively.

Key words:

1. [1]
  1 WANG Xing-Tian. Inorganic Chemicals Industry, 2011, 43(3): 1-71 WANG Xing-Tian. Inorganic Chemicals Industry, 2011, 43(3): 1-7
2. [2]
  王杏田. 无机盐工业, 2011, 43(3): 1-7王杏田. 无机盐工业, 2011, 43(3): 1-7
3. [3]
  2 MU Qi-Dao. Chemical Reagents, 2002, 24(3): 142-1452 MU Qi-Dao. Chemical Reagents, 2002, 24(3): 142-145
4. [4]
  穆启道. 化学试剂, 2002, 24(3): 142-145穆启道. 化学试剂, 2002, 24(3): 142-145
5. [5]
  3 Sauvage L, Frank D, Stearne J, Millikan M B. Anal. Chim. Acta, 2002, 458(1): 223-2303 Sauvage L, Frank D, Stearne J, Millikan M B. Anal. Chim. Acta, 2002, 458(1): 223-230
6. [6]
  4 Sohrin Y, Urushihara S, Nakatsuka S, Kono T, Higo E, Minami T, Norisuye K, Umetani S. Anal. Chem., 2008, 80 (16): 6267-62734 Sohrin Y, Urushihara S, Nakatsuka S, Kono T, Higo E, Minami T, Norisuye K, Umetani S. Anal. Chem., 2008, 80 (16): 6267-6273
7. [7]
  5 YIN Xue-Bo, ZENG Zhi-Gang, LI San-Zhong, WU Li, WANG Xiao-Yuan, ZHANG Guo-Liang, CHEN Shuai. Chinese J. Anal. Chem., 2011, 39(8): 1228-12325 YIN Xue-Bo, ZENG Zhi-Gang, LI San-Zhong, WU Li, WANG Xiao-Yuan, ZHANG Guo-Liang, CHEN Shuai. Chinese J. Anal. Chem., 2011, 39(8): 1228-1232
8. [8]
  殷学博, 曾志刚, 李三忠, 武力, 王晓媛, 张国良, 陈帅. 分析化学. 2011, 39(8): 1228-1232殷学博, 曾志刚, 李三忠, 武力, 王晓媛, 张国良, 陈帅. 分析化学. 2011, 39(8): 1228-1232
9. [9]
  6 PANG Yan-Hua, LIU Ming-Yang, LIU Shu-Yan, DONG Zhen-Lin. Chinese Journal of Chromatography, 2011, 29(10): 1027-10306 PANG Yan-Hua, LIU Ming-Yang, LIU Shu-Yan, DONG Zhen-Lin. Chinese Journal of Chromatography, 2011, 29(10): 1027-1030
10. [10]
  庞艳华, 刘名扬, 刘淑艳, 董振霖. 色谱, 2011, 29(10): 1027-1030庞艳华, 刘名扬, 刘淑艳, 董振霖. 色谱, 2011, 29(10): 1027-1030
11. [11]
  7 GB/T 1271-2011, Chemical Reagent Potassium Fluoride Dihydrate. National Standards of the People's Republic of China7 GB/T 1271-2011, Chemical Reagent Potassium Fluoride Dihydrate. National Standards of the People's Republic of China
12. [12]
  化学试剂, 二水合氟化钾. 中华人民共和国国家标准, GB/T 1271-2011化学试剂, 二水合氟化钾. 中华人民共和国国家标准, GB/T 1271-2011
13. [13]
  8 XIONG Yu-Di, LIU Xia, FENG Chang-Gen. Spectroscopy and Spectral Analysis, 2008, 28(1): 231-2348 XIONG Yu-Di, LIU Xia, FENG Chang-Gen. Spectroscopy and Spectral Analysis, 2008, 28(1): 231-234
14. [14]
  熊宇迪, 刘霞, 冯长根. 光谱学与光谱分析, 2008, 28(1): 231-234熊宇迪, 刘霞, 冯长根. 光谱学与光谱分析, 2008, 28(1): 231-234
15. [15]
  9 ZHAO Xi-Juan, LI Chun-Mei, HUANG Cheng-Zhi, LI Yuan-Fang. Chinese J. Anal. Chem., 2009, 37(9): 1345-13489 ZHAO Xi-Juan, LI Chun-Mei, HUANG Cheng-Zhi, LI Yuan-Fang. Chinese J. Anal. Chem., 2009, 37(9): 1345-1348
16. [16]
  赵希娟, 李春梅, 黄承志, 李原芳. 分析化学, 2009, 37(9): 1345-1348赵希娟, 李春梅, 黄承志, 李原芳. 分析化学, 2009, 37(9): 1345-1348
17. [17]
  10 ZHU Yan. Principle and Application of Ion Chromatography, Hangzhou: Zhejiang University Press, 200210 ZHU Yan. Principle and Application of Ion Chromatography, Hangzhou: Zhejiang University Press, 2002
18. [18]
  朱岩. 离子色谱原理及其应用. 杭州: 浙江大学出版社, 2002朱岩. 离子色谱原理及其应用. 杭州: 浙江大学出版社, 2002
19. [19]
  11 Kaiser E, Rohrer J S, Jensen D. J. Chromatogr. A, 2001, 920(1-2): 127-13311 Kaiser E, Rohrer J S, Jensen D. J. Chromatogr. A, 2001, 920(1-2): 127-133
20. [20]
  12 Vermeiren K. J. Chromatogr. A, 2005, 1085(1): 66-7312 Vermeiren K. J. Chromatogr. A, 2005, 1085(1): 66-73
21. [21]
  13 Ayushi, Kumar S D, Reddy A V R. J. Chromatogr. Sci., 2012, 50 (1): 81-8313 Ayushi, Kumar S D, Reddy A V R. J. Chromatogr. Sci., 2012, 50 (1): 81-83
22. [22]
  14 Zhong Y, Zhou W, Zhu H, Zeng X, Ye M, Zhang P, Zhu Y. Anal. Chim. Acta, 2011, 686(1-2): 1-814 Zhong Y, Zhou W, Zhu H, Zeng X, Ye M, Zhang P, Zhu Y. Anal. Chim. Acta, 2011, 686(1-2): 1-8
23. [23]
  15 Hu Z, Chen H, Yao C, Zhu Y. J. Chromatogr. Sci., 2011, 49(8): 617-62115 Hu Z, Chen H, Yao C, Zhu Y. J. Chromatogr. Sci., 2011, 49(8): 617-621
24. [24]
  16 HU Zhen-Zhen, WANG Lei, YAO Chao-Ying, ZHU Yan, ZHANG Pei-Min. Chinese J. Anal. Chem., 2011, 39(8): 1261-126516 HU Zhen-Zhen, WANG Lei, YAO Chao-Ying, ZHU Yan, ZHANG Pei-Min. Chinese J. Anal. Chem., 2011, 39(8): 1261-1265
25. [25]
  胡真真, 王雷, 姚超英, 朱岩, 张培敏. 分析化学, 2011, 39(8): 1261-1265胡真真, 王雷, 姚超英, 朱岩, 张培敏. 分析化学, 2011, 39(8): 1261-1265
26. [26]
  17 MOU Shi-Fen, LIU Ke-Na, DING Xiao-Jing. Ion Chromatography Method and Application. Beijing: Chemical Industry Press, 2005: 110-11217 MOU Shi-Fen, LIU Ke-Na, DING Xiao-Jing. Ion Chromatography Method and Application. Beijing: Chemical Industry Press, 2005: 110-112
27. [27]
  牟世芬, 刘克纳, 丁晓静. 离子色谱方法及应用. 北京: 化学工业出版社, 2005: 110-112牟世芬, 刘克纳, 丁晓静. 离子色谱方法及应用. 北京: 化学工业出版社, 2005: 110-112
28. [28]
  18 Dionex Corporation, Product Manual for IonPac ICE-AS6. Rev.07. Sunnyvale, CA. Document No. 034961, 2005. http://www.dionex.com/en-us/webdocs/4453-34961-07_ICE_AS6_Manual_V26.pdf18 Dionex Corporation, Product Manual for IonPac ICE-AS6. Rev.07. Sunnyvale, CA. Document No. 034961, 2005. http://www.dionex.com/en-us/webdocs/4453-34961-07_ICE_AS6_Manual_V26.pdf

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 487
HTML全文浏览量: 41

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

离子色谱柱切换法测定氟化盐高纯试剂中的阴离子杂质

通讯作者: 胡忠阳

English

Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching

Corresponding author: 胡忠阳

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

离子色谱柱切换法测定氟化盐高纯试剂中的阴离子杂质

通讯作者: 胡忠阳

English

Determination of Impurity Anions in High Pure Fluoride Reagents by Ion Chromatography with Column-Switching

Corresponding author: 胡忠阳

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs