Abstract：As common impurity elements in high-purity quartz, Li, Be, B and Na have important influence on the product performance. Therefore, it is necessary to establish the corresponding determination method. A method for the determination of nine impurity elements (including Li, Be, B, Na, Mg, Al, S, Ti and Cu) in high-purity quartz by direct-current glow discharge mass spectrometry (dc-GDMS) was developed using germanium mask as the secondary cathode in experiments. The thickness of germanium mask used was 0.25 mm, and there were four slits with size of 1 mm×8 mm. The spacing between two slits was 1 mm. The influence of glow discharge parameters on matrix signal intensity, signal stability and the signal ratio of matrix to germanium mask was investigated. The experiments showed that when the discharge parameter was 1.3 mA/1 350 V, the signal intensity of matrix (28Si) could reach 1.3×109 cps. The discharge was stable, and the signal ratio of matrix to germanium mask was 1∶40. The contents of Li, Be, B, Na, Mg, Al, S, Ti and Cu in high-purity quartz sample were determined according to the experimental method. The relative standard deviations (RSD, n=5) of results were all within 30%. The effects of germanium mask and tantalum mask on the testing result of high-purity quartz were also compared. The results showed that due to the high content of Cu in tantalum mask, the determination result of Cu had great difference, while the determination results of other elements were basically consistent. Meanwhile, the detection limits of impurity elements in high-purity quartz with germanium mask could reach the ng/g level, which were lower than those using tantalum mask.
谭秀珍, 李江霖, 李瑶, 邓育宁, 朱刘. 锗二次阴极-直流辉光放电质谱法测定高纯石英中9种杂质元素[J]. 冶金分析, 2022, 42(11): 24-29.
TAN Xiuzhen, LI Jianglin, LI Yao, DENG Yuning, ZHU Liu. Determination of nine impurity elements in high-purity quartz by direct-current glow discharge mass spectrometry using germanium as secondary cathode. , 2022, 42(11): 24-29.
[1] 杨晓勇,孙超,曹荆亚,等.高纯石英的研究进展及发展趋势[J].地学前缘,2022,29(1):231-244. YANG Xiaoyong,SUN Chao,CAO Jingya,et al.High purity quartz: Research progress and perspective review[J].Earth Science Frontiers,2022,29(1):231-244. [2] 张宏丽,倪文山,刘磊,等.冷焰模式-电感耦合等离子体质谱法测定高纯石英中痕量铁[J].冶金分析,2021,41(7):28-24. ZHANG Hongli,NI Wenshan,LIU Lei,et al.Determination of trace ion in high-purity quartz by cool flame mode-inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2021,41(7):28-24. [3] 陈永康,杨静,张笑旻,等.ICP-AES法测定二氧化硅标准物质中微量杂质元素的研究[J].化学工程师,2017(5):22-26. CHEN Yongkang,YANG Jing,ZHANG Xiaomin,et al.Study on the determination of trace impurities in silicon dioxide reference material by ICP-AES[J].Chemical Engineer,2017(5):22-26. [4] 张萍,符靓,刘宏伟.直流辉光放电质谱法测定海绵钛中杂质元素[J].冶金分析,2016,36(8):7-12. ZHANG Ping,FU Liang,LIU Hongwei.Determination of impurity elements in titanium sponge by direct current glow discharge mass spectrometry[J].Metallurgical Analysis,2016,36(8):7-12. [5] Sabatino M D.Detection limits for glow discharge mass spectrometry (GDMS) analyses of impurities in solar cell silicon[J].Measurement,2014,50:135-140. [6] Hoffmann V, Kasik M,Robinso P K,et al.Glow discharge mass spectrometry[J].Anal. Bioanal. Chem.,2005,381:173-188. [7] Bogaerts A,Gijbels R.New developments and applications in GDMS[J].Fresenius J.Anal.Chem.,1999,364(5):367-375. [8] Venzago C,Weigert M.Application of the glow discharge mass spectrometry (GDMS) for the multi-element trace and ultratrace analysis of sputtering targets[J].Fresenius J.Anal.Chem.,1994,350:303-309. [9] Yang J,Shin H,Jung S,et al.Quantitative analysis of impurities in gallium metal using RSF calculated by analyzing aluminum matrix CRMs using glow discharge mass spectrometry[J].MAPAN-Journal of Metrology Society of India,2021,36:813-819. [10] 刘元元,胡净宇.辉光放电质谱法测定棒状高纯镁中12种杂质元素[J].冶金分析,2018,38(4):16-21. LIU Yuanyuan,HU Jingyu.Determination of twelve impurities in rodlike high-purity magnesium by glow discharge mass spectrometry[J].Metallurgical Analysis,2018,38(4):16-21. [11] 谭秀珍,李瑶,林乾彬,等.直流辉光放电质谱分析导体和非导体样品的高纯铟片制样方法研究[J].冶金分析,2018,38(9):1-7. TAN Xiuzhen,LI Yao,LIN Qianbin,et al.Investigation on sample preparation method of high purity indium sheet in analysis of conductor and non-conductor sample by direct current glow discharge mass spectrometry[J].Metallurgical Analysis,2018,38(9):1-7. [12] Kurochkin V D,Kravchenko L P.Aanlysis of impurities in high-purity aluminum oxide by glow discharge mass spectrometry[J].Powder Metallurgy and Metal Ceramics,2006,45:9-10. [13] 谭秀珍,李瑶,林乾彬,等.直流辉光放电质谱法测定高纯二氧化锗中的16种杂质元素及其相对灵敏度因子的求取[J].理化检验(化学分册),2019,55(7):859-864. TAN Xiuzhen,LI Yao,LIN Qianbin,et al.Determination of 16 impurity-elements in high purity germanium dioxide by dc-GDMS and evaluation of their relative sensitivity factors[J].Physical Testing and Chemical Analysis (Part B: Chemical Analysis),2019,55(7):859-864. [14] 胡芳菲,王长华,李继东.直流辉光放电质谱法测定高纯氧化镧中25种杂质元素[J].冶金分析,2014,34(3):24-29. HU Fangfei,WANG Changhua,LI Jidong.Determination of twenty-five impurity elements in high purity lanthanum oxide by direct current glow discharge mass spectrometry[J].Metallurgical Analysis,2014,34(3):24-29. [15] Battagliarin M,Sentimenti E,Scattolin R,et al.An innovative sample preparation procedure for trace and ultra-trace analysis on non-conducting powders by direct current glow discharge mass spectrometry[J].Spectrochimia Acta,1995,50B(1):13-25. [16] QIAN Rong,ZHUO Shangjun,WANG Zheng,et al. Direct current glow discharge mass spectrometric analysis of non-conducting materials using a surface coating method[J].Journal of Analytical Atomic Spectrometry,2013,28:1061-1067. [17] SIQIN Bilige,QIAN Rong,ZHUO Shangjun,et al.Studies of rare earth elements to distinguish nephrite samples from different deposits using direct current glow discharge mass spectrometry[J].J.Anal.At.Spectrom.,2014,29:2064-2071. [18] DONG Jiangli,QIAN Rong,ZHUO Shangjun,et al.Development and application of a porous cage carrier method for detecting trace elements in soils by direct current glow discharge massspectrometry[J].J. Anal. At. Spectrom.,2019,34:2244-2251. [19] 谭秀珍,李瑶,朱刘,等.不同制样方法对直流辉光放电质谱法测定氮化硼中27种杂质元素的影响[J].冶金分析,2019,39(8):23-29. TAN Xiuzhen,LI Yao,ZHU Liu,et al.Effect of sample preparation method on the determination of twenty seven impurity elements in boron nitride by direct current glow discharge masss pectrometry[J].Metallurgical Analysis,2019,39(8):23-29. [20] Milton D M P,Hutton R C.Investigations into the suitability of using a secondary cathode to analysis glass using glow discharge mass spectrometry[J].Spectrochimica Acta,1993,48B(1):39-52. [21] Schelles W,Gendt S D,Van Grieken R E.Optimization of secondary cathode thickness for direct current glow discharge mass spectrometric analysis of glass[J].Journal of Analytical Atomic Spectrometry,1996,11:937-941. [22] Schelles W,Van Grieken R E.Direct current glow discharge mass spectrometric analysis of macor ceramic using a secondary cathode[J].Anal. Chem.,1996,68:3570-3574. [23] Busam J, Stokkan G, Muggerud A M F, et al. Application of 7 N In as secondary cathode for the direct current-glow discharge mass spectrometry analysis of solid, fused high-purity quartz[J]. J.Mass Spectrom.,2021,56:1-8. [24] Busam J,Paudel G,Sabatino M D.Silicon and indium as secondary cathodes for the analysis of solid alumina and sapphire by slow-flow direct-current glow discharge mass spectrometry[J].J.Anal.At.Spectrom.,2022,37:172-177.
