电感耦合等离子体-质谱法测定高纯四甲基氢氧化铵中超痕量金属元素  

Ultra-trace Metal Elements Analysis of High Purity Tetramethylammonium Hydroxide Using Inductively Coupled Plasma Tandem Mass Spectrometry

作　　者：符靓 施树云[2] 陈晓青[2] FU Liang;SHI Shu-Yun;CHEN Xiao-Qing(Collaborative Innovation Center of Green Development for Wuling Mountain Areas,Yangtze Normal University, Chongqing 408100, China;School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, 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,重庆408100 [2]中南大学化学化工学院,长沙410083

出　　处：《分析化学》2018年第1期107-112,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.21275163);重庆市科委前沿与应用基础研究项目(No.cstc2015jcyj A10038);重庆市教委重点科研项目(No.KJ1601224)资助~~

摘　　要：建立了高纯四甲基氢氧化铵(TMAH)中超痕量金属元素的分析方法。25%(w/w)高纯TMAH溶液样品经超纯水稀释后直接进样,应用电感耦合等离子体串联质谱(ICP-MS/MS)法测定其中12种超痕量金属元素。在MS/MS模式下,分别向碰撞/反应池(CRC)中加入O_2和NH_3-He(1∶9,V/V),消除质谱干扰,采用O_2质量转移法对Cr、Mn、Ni和Mo进行测定,O_2原位质量法对Cd和Pb进行测定,NH_3质量转移法对Fe、Co、Cu和Zn进行测定,NH_3原位质量法对Mg和Al进行测定。12种金属元素的检出限为0.3~57.2 ng/L,加标回收率在92.0%~106.0%之间,相对标准偏差(RSD)≤4.6%,表明本方法具有良好的准确性和精密度。本方法已成功应用于25%高纯TMAH溶液中超痕量金属元素的分析。An analytical method was proposed to determine the ultra-trace metal elements in high-purity tetramethylammonium hydroxide(TMAH).A total of12kinds of ultra-trace metal elements in25%(w/w)high-purity TMAH aqueous solution were directly determined after simple dilution with ultrapure water by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS).In MS/MS mode,the spectral interferences were eliminated by the reaction of target ions with O2or NH3/He(1:9,V/V)in the collision/reaction cell(CRC)of the ICP-MS/MS.Cr,Mn,Ni and Mo were determined using the O2mass shift method.Cd and Pb were analyzed based on the O2on-mass method.Fe,Co,Cu and Zn were determined using the NH3/He mass shift method.Mg and Al were determined using the NH3/He on-mass.The detection limits for analytes were in the range of0.3-57.2ng/L.The spiked recoveries were in range of92.0%-106.0%,and the relative standard deviations(RSDs)were less than or equal to4.6%.The procedure was applied for determining ultra-trace metal elements in25%high-purity TMAH aqueous solution.

关 键 词：四甲基氢氧化铵 电感耦合等离子体串联质谱 金属元素 质量转移法 原位质量法 

分 类 号：O657.63[理学—分析化学] TQ207.4[理学—化学]