气体吸收-电感耦合等离子体三重四极杆质谱(ICP-MS/MS)法测定电子工业高纯氩气中44种超痕量元素  

Determination of 44 Ultratrace Elements in High-purity Argon in the Electronic Industry by Gas Absorption-Inductively Coupled Plasma Triple Quadrupole Mass Spectrometry(ICP-MS/MS)

作　　者：陈婷婷 李鹰 徐岳 俞晓峰 吴智威 CHEN Tingting;LI Ying;XU Yue;YU Xiaofeng;WU Zhiwei(Hangzhou Puyu Technology Co.,Ltd.,Hangzhou,Zhejiang 311300,China)

机构地区：[1]杭州谱育科技发展有限公司,杭州311300

出　　处：《中国无机分析化学》2024年第7期963-972,共10页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2021YFF0700804)。

摘　　要：随着电子工业对特气纯度要求的日益提高,为能达到更低的检测下限,在国家标准方法的基础上优化气体吸收装置,并使用电感耦合等离子体三重四极杆质谱(ICP-MS/MS)法同时测定特气中44种元素含量。高纯氩气中的超痕量杂质元素可经优化后的气体吸收装置被完全吸收至5%硝酸吸收液中,吸收液可直接经ICP-MS/MS测定,并通过Std、He、NH_(3)、Cool、Cool NH_(3)等多种分析模式,有效消除了目标元素所遭受的多类型质谱干扰(多原子离子、双电荷、同量异位素等)。在优化的实验条件下,采样体积为89.4 L时,高纯氩气中44种超痕量杂质元素可获得的检出限为0.00002~0.0026 ng/L,较国家标准(GB/T 34972—2017)所规定的检出限范围低1~4个数量级,且所有目标元素均可获得优于0.999的标准曲线相关系数,加标回收率为90.1%(Zn)~118%(Na),相对标准偏差在0.68%(Cs)~14%(Zn)。优化后的气体吸收装置具有便携高效、功能多样、隔绝污染等特点,与ICP-MS/MS相结合实现了高纯氩气中超痕量杂质元素的稳定可靠测试,可为半导体、高纯材料等对气体纯度有极高要求的工业产品原料质控提供技术支持。With the increasing demand for purity of special gas in electronics industry,in order to achieve a lower detection limit,the gas absorption device was optimized on the basis of national standard methods,and the inductively coupled plasma triple quadrupole mass spectrometry(ICP-MS/MS)method was used to simultaneously determine 44 elements in special gas.Ultra-trace impurity elements in high purity argon were completely absorbed into 5%nitric acid absorption solution by optimized gas absorption device,which can be directly determined by ICP-MS/MS.Multiple types of mass spectrum interference(multi-atomic ions,double charges,isobaric elements,etc.)suffered by target elements were effectively eliminated through various analysis modes such as Std,He,NH_(3),Cool,Cool NH_(3),etc.Under optimized experimental conditions,when the sampling volume was 89.4 L,the detection limit of 44 ultra-trace impurity elements in high purity argon was 0.00002-0.0026 ng/L,which was 1—4 orders of magnitude lower than the detection limit stipulated by the national standard(GB/T 34972—2017).The standard curve correlation coefficients were better than 0.999 for all target elements.The spiked recovery rates were 90.1%(Zn)—118%(Na),and the relative standard deviations were 0.68%(Cs)—14%(Zn).The optimized gas absorption device has the characteristics of portability,high efficiency,various functions,pollution isolation,etc.Combined with ICP-MS/MS,it realizes stable and reliable testing of ultra-trace impurity elements in high purity argon,and can provide technical support for raw material quality control of industrial products such as semiconductors and high purity materials,which have high requirements for gas purity.

关 键 词：电子特气 超痕量元素 ICP-MS/MS 气体吸收 干扰消除 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]