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

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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

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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？

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通讯作者: 陈斌, bchen63@163.com

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