辉光放电质谱（GDMS）法校正高纯氧化铋中19种元素的相对灵敏度因子  

Calibration on the Relative Sensitivity Factors of Nineteen Elements in High Purity Bismuth Oxide by Glow Discharge Mass Spectrometry

作　　者：谭秀珍 李瑶 陈晶晶 朱刘 邓育宁 TAN Xiuzhen;LI Yao;CHEN Jingjing;ZHU Liu;DENG Yuning(Guangdong First Rare Materials Co.,Ltd.,National Engineering and Technology Research Center of Scattered Metal,Qingyuan,Guangdong 511875,China;Qingyuan First Materials 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]清远先导材料有限公司,广东清远511517

出　　处：《中国无机分析化学》2019年第6期63-68,共6页Chinese Journal of Inorganic Analytical Chemistry

摘　　要：采用标准溶液加入法往高纯氧化铋中加入混合标准溶液,烘干并研磨均匀,制备了5个高纯氧化铋的控制样品。再挑取适量的粉末样品压在高纯铟薄片上,建立了辉光放电质谱(GDMS)法校正高纯氧化铋中的Mg、Al、Ca等19种元素相对灵敏度因子的方法。实验考察了放电参数和制样面积对基体信号强度和稳定性的影响,优化后的辉光放电电流为1.8 mA,放电电压为950 V,压在铟薄片上的高纯氧化铋直径约为6~8 mm。通过选择合适的同位素,在4000的中分辨率下测定即可消除质谱干扰。为了验证加标回收的准确性,采用电感耦合等离子体质谱(ICP-MS)法对控制样品进行测定,所有元素的加标回收率都在80%以上。采用GDMS法测定5个控制样品并结合ICP-MS法的测定值建立工作曲线,大部分元素的线性均达到0.995以上;除Al、Ga、Sb外,大部分元素的校准相对灵敏度因子(calRSF)和仪器自带的标准相对灵敏度因子(stdRSF)的比值都在1/2~2之间,说明GDMS的半定量分析不会有数量级的差别。但对于某些需要准确测定纯度的定量分析,则必须采用基体相匹配的RSF值进行校正。Adopting a standard solution addition method,a mixed standard solution was added to the high-purity Bi 2O 3,dried and mixed well,five control samples of high purity Bi 2O 3 were prepared.Then pressed a proper amount of powder sample on high purity In sheet,a method for calibration the relative sensitivity factors of 19 elements(including Mg,Al,Ca and so on)were established.The influence of discharge parameters and sample preparation area on sensitivity and stability of matrix signal were investigated,the optimized discharge current was 1.8 mA,discharge voltage was 950 V,and the diameter of Bi 2O 3 pressed on in sheet was about 6—8 mm.The mass spectrometry interference could be eliminated under moderate resolution(R=4000)by selecting the proper isotopes.The control samples were tested by inductively coupled plasma mass spectrometry(ICP-MS)to verify their accuracy,and the recovery of all elements was above 80%.Five control samples were analyzed by GDMS and working curve for each elements were established by combining the measured values of ICP-MS,the linear coefficients of most elements were above 0.995;the Cal RSF values obtained by calibration curve were compared with values derived from standard RSF of the instrument,for most elements,the ratio was between 1/2—2 except for Al,Ga,Sb,which indicates that there is no difference of orders of magnitude in semi-quantitative analysis by GDMS.But when the impurities were need to be measured accurately,the RSF values which were obtained by matrix-matched calibration were necessary.

关 键 词：辉光放电质谱仪(GDMS) 高纯氧化铋 控制样品 相对灵敏度因子 

分 类 号：O657.32[理学—分析化学] TH843[理学—化学]