电感耦合等离子体串联质谱准确测定软磁铁氧体粉料中的有害和掺杂元素  

Accurate Determination of Harmful and Doping Elements in Soft Magnetic Ferrite Powders Using Inductively Coupled Plasma Tandem Mass Spectrometry

作　　者：符靓 施树云[2] 马俊才[3] FU Liang;SHI Shu-Yun;MA Jun-Cai(Collaborative Innovation Center of Green Development for Wuling Mountain Areas,Yangtze Normal University,Fuling 408100,China;School of Chemistry and Chemical Engineering,Central South University,Changsha 410083,China;Chongqing Shangjia Electronics Co.,Ltd.,Fuling 408100,China)

机构地区：[1]长江师范学院武陵山片区绿色发展协同创新中心,涪陵408100 [2]中南大学化学化工学院,长沙410083 [3]重庆上甲电子股份有限公司,涪陵408100

出　　处：《分析化学》2019年第9期1382-1389,共8页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.21275163);重庆市科委技术创新与应用示范项目(No.cstc2018jscx-msyb0675)资助~~

摘　　要：提出了在电感耦合等离子体串联质谱(ICP-MS/MS)的MS/MS模式下利用混合反应气消除软磁铁氧体粉料分析中质谱干扰的新策略。选择HNO3-HCl为混合消解试剂,软磁铁氧体粉料样品经微波消解后,采用ICP-MS/MS测定有害元素Na、Mg,以及掺杂元Al、K、Ti和Co。采用混合反应气NH3/He/H2,在MS/MS模式下通过质量转移法和原位质量法消除干扰。研究结果表明,所有分析元素均获得了低背景等效浓度和高灵敏度测定,检出限分别为17 ng/L(Na)、3.1 ng/L(Mg)、5.4 ng/L(Al)、11 ng/L(K)、0.64 ng/L(Ti)和0.53 ng/L(Co)。利用扇形磁场电感耦合等离子体质谱(SF-ICP-MS)对所建立的方法进行评价,在95%置信水平上,两种分析方法的测定值无显著差异,表明所建立的方法准确可靠。本方法简单快速,可无干扰地测定软磁铁氧体粉料中的Na、Mg、Al、K、Ti、Co,为软磁铁氧体粉料中有害和掺杂元素的质量控制提供了新的技术手段。A new strategy for eliminating mass spectral interference in analysis of soft magnetic ferrite powders by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)in the MS/MS mode using mixed reaction gases was proposed.The mixture of nitric acid and hydrochloric acid was used for digesting the samples by a microwave-based digestion system.The contents of harmful elements(Na and Mg)and doping elements(Al,K,Ti and Co)in the digestion solution were determined by ICP-MS/MS.For interferences of mass spectrum in the complex matrix composition of different soft magnetic ferrite powders,in the MS/MS mode,the interferences were eliminated using mixed reaction gases of NH3/He/H2 through mass shift and on-mass methods.The limits of detection for Na,Mg,Al,K,Ti and Co were 17,3.1,5.4,11,0.64 and 0.53 ng/L,respectively.The developed method was evaluated by sector field ICP-MS(SF-ICP-MS),and there was no significant difference between the two analytical methods at a 95%confidence level,indicating that the developed method was accurate and reliable.This method was demonstrated simple and quick,and could be used in interference-free determination of Na,Mg,Al,K,Ti and Co in soft magnetic ferrite powders,which provided a new technical means for quality control of harmful and doping elements in soft magnetic ferrite powders.

关 键 词：软磁铁氧体粉料 电感耦合等离子体串联质谱 有害元素 掺杂元素 混合反应气 

分 类 号：TM2[一般工业技术—材料科学与工程]