电感耦合等离子体串联质谱法测定钽酸锂中金、钠、钾和钙的含量

引用本文: 墨淑敏, 祝利红, 李爱嫦, 李娜, 陈雄飞. 电感耦合等离子体串联质谱法测定钽酸锂中金、钠、钾和钙的含量[J]. 分析化学, 2021, 49(2): 246-252. doi: 10.19756/j.issn.0253-3820.201404 shu

Citation: MO Shu-Min, ZHU Li-Hong, LI Ai-Chang, LI Na, CHEN Xiong-Fei. Determination of Gold, Sodium, Potassium and Calcium in Lithium Tantalate by Inductively Coupled Plasma-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2021, 49(2): 246-252. doi: 10.19756/j.issn.0253-3820.201404 shu

电感耦合等离子体串联质谱法测定钽酸锂中金、钠、钾和钙的含量

国标(北京)检验认证有限公司, 北京 100088

通讯作者: 墨淑敏,E-mail:msmustb@126.com

基金项目:
工信部"国家新材料测试评价平台-主中心"项目（No.52801）资助。

摘要: 常规单杆电感耦合等离子质谱（ICP-QMS）测定钽酸锂中Au、Na、K、Ca时，质谱干扰严重，其中，Au的定量分析完全无法进行。本研究建立了电感耦合等离子体串联质谱（ICP-MS/MS）测定钽酸锂中Au、Na、K、Ca含量的方法，对反应原理进行了研究，对测定参数进行了优化。选择¹³³Cs为内标校正基体效应。在两种模式（O₂流速0.9 mL/min，m/z=197原位质量模式；NH₃/He流速6.5 mL/min，m/z=231质量转移模式）下，以Au（NH₃）₂⁺离子团形式测定Au。Na在O₂原位模式与NH₃原位模式的测定结果无显著差异，验证了基体Li的氧化物干扰可忽略不计。本方法对Au、Na、K、Ca的检出限在0.006~0.11 μg/g范围内，样品测定结果的相对标准偏差（RSD，n=7）小于10%，加标回收率为86.3%~106.5%。

关键词:

English

Determination of Gold, Sodium, Potassium and Calcium in Lithium Tantalate by Inductively Coupled Plasma-Tandem Mass Spectrometry

Guobiao(Beijing) Testing & Certification Co., Ltd., Beijing 100088, China

Corresponding author: MO Shu-Min, msmustb@126.com

Received Date: 11 July 2020
Revised Date: 13 December 2020
Fund Project:
Supported by the Ministry of Industry and Information Technology (National New Material Testing and Evaluation Platform-Main Center Project) (No.52801).

Abstract: The interferences of gold, sodium, potassium and calcium are serious in the determination of lithium tantalate by conventional quadrupole inductively coupled plasma mass spectrometry (ICP-QMS), especially for gold. In this study, the methods for determination of gold, sodium, potassium and calcium in lithium tantalate by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) were developed. The reaction principles were studied and the determination parameters were optimized. ¹³³Cs was selected as internal standard to compensate matrix effect. Au could be detected at m/z=197 under on-mass mode with 0.9 mL/min O₂ as reaction gas, or detected at m/z=231 as Au(NH₃)₂⁺ cluster ion under mass-shift mode with 6.5 mL/min NH₃/He mixture as reaction gas. There was no significant difference between the detection results of Na under O₂ or NH₃ on-mass mode, which verified that the interference of LiO was negligible. The detection limits of Au, Na, K and Ca were 0.006-0.11 μg/g. The relative standard deviations (RSDs, n=7) of sample detection results were less than 10%, and the recoveries were 86.3%-106.5%.

Key words:

Lithium tantalite
/ Inductively coupled plasma-tandem mass spectrometry
/ Gold
/ On-mass
/ Mass-shift

1. [1]
  LIANG Jin-Ling, ZHANG Yun, QIU Xiao-Yan, WU Sheng-Yu, LUO Ya. Acta Phys. Sin., 2019, 68(20):137-144. 梁金铃, 张耘, 邱晓燕, 吴圣钰, 罗娅. 物理学报, 2019, 68(20):137-144.
2. [2]
  MASLOBOEVA S M, PALATNIKOV M N, ARUTYUNYAN L G. Inorg. Mater., 2020, 56(3):270-276.
3. [3]
  PALATNIKOV M N, SHCHERBINA O B, MASLOBOEVA S M, EFREMOV V V. Russ. J. Inorg. Chem., 2020, 65(3):440-445.
4. [4]
  YS/T 898-2013, Methods for Chemical Analysis of the High Purity Tantalum-Determination of Trace Impurity Element Content-Inductively Coupled Plasma Mass Spectrometry. Non Ferrous Metal Industry Standard of the People's Republic of China. 高纯钽化学分析方法痕量杂质元素的测定电感耦合等离子体质谱法.中华人民共和国有色金属行业标准. YS/T 898-2013.
5. [5]
  LYU Ting, TAO Mei-Juan. Anal. Instrum., 2020, (2):48-54. 吕婷, 陶美娟. 分析仪器, 2020, (2):48-54.
6. [6]
  LIU Ting, BAI Huan-Huan, LEI Xiao-Yan, LUO Ce, LI Jian. Phys. Test. Chem. Anal. Part B, 2017, 53(4):451-455. 刘婷, 白焕焕, 雷小燕, 罗策, 李剑. 理化检验-化学分册, 2017, 53(4):451-455.
7. [7]
  GB/T 15076.1-2017, Methods for Chemical Analysis of Tantalum and Niobium-Part 1:Determination of Tantalum Content in Niobium-Inductively Coupled Plasma Aatomic Emission Spectrometry. National Standards of the People's Republic of China. 钽铌化学分析方法第1部分:铌中钽量的测定电感耦合等离子体原子发射光谱法. 中华人民共和国国家标准. GB/T 15076.1-2017
8. [8]
  CHEN Gang, GE Ai-Jing, ZHUO Shang-Jun, WANG Pei-Ling. J. Chin. Mass Spectrom. Soc., 2007, 28(1):36-39. 陈刚, 葛爱景, 卓尚军, 王佩玲. 质谱学报, 2007, 28(1):36-39.
9. [9]
  YS/T 899-2013, Methods for Chemical Analysis of High Purity Tantalum-Determination of Trace Impurity Element Content-Glow Discharge Mass Spectrometry. Non Ferrous Metal Industry Standard of the People's Republic of China. 高纯钽化学分析方法痕量杂质元素的测定辉光放电质谱法. 中华人民共和国有色金属行业标准. YS/T 899-2013.
10. [10]
  ZHOU Xue-Zhong, LIU Hong-Wei. Spectrosc. Spect. Anal., 2018, 38(11):3567-3571. 周学忠, 刘宏伟. 光谱学与光谱分析, 2018, 38(11):3567-3571.
11. [11]
  CHEN Wen, FAN Xiao-Wei, GUO Cai-Nv, SONG Xu-Dong, LIU Yi-Qiang, XU Na. Chin. J. Anal. Chem., 2019, 47(3):403-409. 陈文, 樊小伟, 郭才女, 宋旭东, 刘宜强, 徐娜. 分析化学, 2019, 47(3):403-409.
12. [12]
  DIEZ-FERNÁNDEZ S, JAEGLER H, BRESSON C, CHARTIER F, EVRARD O, HUBERT A, NONELL A, POINTURIER F, ISNARD H. Talanta, 2020, 206:120221.
13. [13]
  CHAINET F, DESPREZ A, CARBONNEAUX S, AYOUNI L, MILLIAND M L, LIENEMANN C P. Fuel Process. Technol., 2019, 1881(6):60-69.
14. [14]
  CAO L G, ZHENG J, TSUKADA H, PAN S M, WANG Z T, TAGAMI K, UCHIDA S. Talanta, 2016, 159(10):55-63.
15. [15]
  LIN Chun-Hua, XIE Xian-Qing, LIU De-Yong, QIU Chun-Xin, LIAO Wei-Lin, SONG Yong-Hai. J. Anal. Sci., 2018, 34(5):596-600. 林春花, 谢贤清, 刘德永, 邱春新, 廖维林, 宋永海. 分析科学学报, 2018, 34(5):596-600.
16. [16]
  LIU Yuan-Yuan, HU Jing-Yu. Chin. Metall. Anal., 2018, 38(5):1-6. 刘元元, 胡净宇. 冶金分析, 2018, 38(5):1-6.
17. [17]
  JIANG Bo, HUANG Jian-Hua. Spectrosc. Spect. Anal., 2018, 38(9):2937-2942. 江波, 黄建华. 光谱学与光谱分析, 2018, 38(9):2937-2942.
18. [18]
  LI Ai-Yang, WU Su-Yun, LIU Ning, LIU Shui-Lin. Food Ferment. Ind., 2020, 46(9):260-264. 李爱阳, 伍素云, 刘宁, 刘水林. 食品与发酵工业, 2020, 46(9):260-264.
19. [19]
  FU Liang, SHI Shu-Yun, MA Jun-Cai. Chin. J. Anal. Chem., 2019, 47(9):1382-1389. 符靓, 施树云, 马俊才. 分析化学, 2019, 47(9):1382-1389.
20. [20]
  ZHU X W, HE Q, XU F J, MA X X, XING Z, ZHANG S C, ZHANG X R. J. Anal. Atom. Spectrom., 2020, 35(4):804-809.

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 18
HTML全文浏览量: 1

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

电感耦合等离子体串联质谱法测定钽酸锂中金、钠、钾和钙的含量

通讯作者: 墨淑敏,E-mail:msmustb@126.com

English

Determination of Gold, Sodium, Potassium and Calcium in Lithium Tantalate by Inductively Coupled Plasma-Tandem Mass Spectrometry

Corresponding author: MO Shu-Min, msmustb@126.com

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

电感耦合等离子体串联质谱法测定钽酸锂中金、钠、钾和钙的含量

通讯作者: 墨淑敏,E-mail:msmustb@126.com

English

Determination of Gold, Sodium, Potassium and Calcium in Lithium Tantalate by Inductively Coupled Plasma-Tandem Mass Spectrometry

Corresponding author: MO Shu-Min, msmustb@126.com

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