直流辉光放电质谱法测定高纯α-Al 2 O 3颗粒中16种杂质元素  

Analysis of Sixteen Impurity Elements in High-purityα-Al 2 O 3 Particle by Direct-current Glow Discharge Mass Spectrometry

作　　者：谭秀珍 李江霖 李瑶 邓育宁 朱刘 TAN Xiuzhen;LI Jianglin;LI Yao;DENG Yuning;ZHU Liu(National Engineering and Technology Research Center of Scattered Metal,Guangdong First Rare Materials Co.,Ltd.,Qingyuan,Guangdong 511875,China;Vital Thin Film Materials(Guangdong)Co.,Ltd.,Qingyuan,Guangdong 511517,China)

机构地区：[1]广东先导稀材股份有限公司,国家稀散金属工程技术研究中心,广东清远511875 [2]先导薄膜材料(广东)有限公司,广东清远511517

出　　处：《中国无机分析化学》2023年第7期755-760,共6页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：采用高纯Ga作为辅助电极,通过考察取样量、放电参数对基体信号强度、信号稳定性、基体和Ga的信号比值的影响,建立了直流辉光放电质谱法(dc-GDMS)测定高纯α-Al_(2)O_(3)颗粒中的Li、Be、Na、Mg等16种杂质元素含量的分析方法。当选取3颗2 mm左右大小的α-Al_(2)O_(3)颗粒用Ga包裹,在1.6 mA/950 V的放电参数下,基体27 Al信号稳定,强度为3.2×10^(8) cps,Al、Ga的信号比约为1∶270。采用实验方法对α-Al_(2)O_(3)颗粒独立测定5次,相对标准偏差均在30%以内。为了验证Ga对α-Al_(2)O_(3)颗粒测定结果的影响,分别采用电感耦合等离子体发射光谱法(ICP-OES)和dc-GDMS法对易于消解的γ-Al_(2)O_(3)粉进行测定。对于dc-GDMS法,选择压在Ga上的γ-Al_(2)O_(3)粉直径约为4~5 mm,在同样的放电参数下,27 Al的信号强度为3.0×10^(9) cps,Al、Ga的信号比约为1∶29。γ-Al_(2)O_(3)粉的GDMS测定结果和ICP-OES基本一致。采用Ga作辅助电极测定α-Al_(2)O_(3)颗粒和γ-Al_(2)O_(3)粉的检出限均可达ng/g。Using the high purity Ga as auxiliary cathode,after investigating the influence of sample amount,glow discharge conditions on matrix intensity,signal stability and the matrix to Ga signal ratio,the determination method for sixteen impurity elements(including Li,Be,Na,Mg and so on)in high-purityα-Al_(2)O_(3) particle was developed by direct-current glow discharge mass spectrometry(dc-GDMS).Threeα-Al_(2)O_(3) particles of about 2 mm size were selected and wrapped with Ga,the discharge current was 1.6 mA,the discharge voltage was 950 V,the matrix(27 Al)intensity could reach 3.2×10^(8) cps,the signal was stable and matrix to Ga signal ratio was about 1∶270.The sample was determined independently for five times,and the relative standard deviations were less than 30%.In order to verify the effect of Ga on the determination results ofα-Al_(2)O_(3) particle,theγ-Al_(2)O_(3) powder,which was easy to be digested,was selected and tested by inductively coupled plasma atomic emission spectrometry(ICP-OES)and dc-GDMS,respectively.For GDMS,the diameter ofγ-Al_(2)O_(3) powder pressed on Ga was about 4—5 mm,under the same discharge parameter,the matrix(27 Al)intensity could reach 3.0×10^(9) cps,and matrix to Ga signal ratio was about 1∶29.The results ofγ-Al_(2)O_(3) powder by GDMS were consistent with those obtained by ICP-OES.Meanwhile,the detection limit of impurity elements in high-purityα-Al_(2)O_(3) particle andγ-Al_(2)O_(3) powder by using high purity Ga as auxiliary cathode both can reach ng/g level.

关 键 词：直流辉光放电质谱仪(dc-GDMS) 高纯Ga 高纯α-Al 2 O 3颗粒 杂质元素 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]