Abstract:Silver, boron and tin occupy a unique place in geochemical sample analysis. But boron is hardly volatilized, while silver and tin can be only determined by emission spectrometry due to the characteristics of volatile property. In the determination process, some factors in pretreatment such as evaporation behavior, tungsten foil and exhaust air volume play an important role on the accurate determination of silver, boron and tin. Potassium pyrosulfate (K2S2O7), sodium fluoride (NaF), aluminum oxide (Al2O3), germanium oxide (GeO2) and carbon powder (C) were used as buffer. Germanium (Ge) was selected as the internal standard. Alternating current (AC) arc emission spectrometry was used for the determination of silver, boron and tin. The factors influencing the determination of silver, boron and tin in geochemical samples were discussed using CCD-1 plane grating arc emission spectrometer. The results showed that the spectral intensity of volatile elements (silver and tin) reached the maximum value at 14 s, while the spectral intensity of involatile element (boron) reached the maximum value at 16 s, the optimal spectrographic time was 30 s; the tungsten foil was polished and the gap was adjusted. The logarithmic deviation (ΔlgC) between the average of the measurement results and certified value and relative standard deviation (RSD, n=6) of national primary certified reference materials (GBW07375, GBW07401 and GBW07312) were 0-0.02 and 2.30%-5.34%, respectively, which could meet the requirements of trueness and precision. When the exhaust air volume was 3/4, the logarithmic deviation between the average and certified value of the measurement results (ΔlgC) and relative standard deviation (RSD, n=6) of national primary certified reference materials (GBW07375, GBW07401 and GBW07312) were 0-0.02 and 1.04%-8.32%, respectively.The trueness and precision of experimental method could meet the requirements,and it can be used to determine silver, boron and tin in geochemical samples.
何涛, 王鹏, 邓攀直, 张振. 平面光栅电弧发射光谱法测定地球化学样品中银硼锡的影响因素探讨[J]. 冶金分析, 2022, 42(10): 63-69.
HE Tao, WANG Peng, DENG Panzhi, ZHANG Zhen. Discussion of influencing factors on the determination of silver, boron and tin in geochemical samples by plane grating arc emission spectrometry. , 2022, 42(10): 63-69.
[1] 岩石矿物分析编写组.岩石矿物分析:第1分册[M].4版.北京:地质出版社,2011:438-449. [2] 岩石矿物分析编写组.岩石矿物分析:第4分册[M].4版.北京:地质出版社,2011:781-788. [3] 张雪梅,张勤.发射光谱法测定勘查地球化学样品中银硼锡钼铅[J].岩矿测试,2006,25(4):323-326. ZHANG Xuemei,ZHANG Qin.Determination of silver,boron,tin,molybdenum and lead in geochemical exploration samples by emission spectrometry[J].Rock and Mineral Analysis,2006,25(4):323-326. [4] 丁春霞,王琳,孙慧莹,等.发射光谱法测定生态地球化学调查样品中的银锡硼[J].黄金,2012,33(10):55-58. DING Chunxia,WANG Lin,SUN Huiying,et al.Determination of sliver,tin and boron in ecological geochemistry samples by emission spectrometry[J].Gold,2012,33(10):55-58. [5] 李亚静,李士杰,唐秀婷,等.CCD-1型平面光栅电弧直读发射光谱法测定化探样品中铅、锡、钼、铜、银、锌[J].中国无机分析化学,2018,8(6):29-35. LI Yajing,LI Shijie,TANG Xiuting,et al.Determination of Pb,Sn,Mo,Cu,Ag and Zn in geochemical exploration samples by CCD-1 plane grating electric arc direct reading emission spectrometer[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(6):29-35. [6] 李超,刘英波,韩豫萍,等.发射光谱测定地球化学物料中的微量银锡硼[J].云南冶金,2018,47(3):84-88. LI Chao,LIU Yingbo,HAN Yuping,et al.The determination of trace amount silver,tin,boron in geochemical materials by emission spectrography[J].Yunnan Metallurgy,2018,47(3):84-88. [7] 姚建贞,郝志红,唐瑞玲,等.固体发射光谱法测定地球化学样品中的高含量锡[J].光谱学与光谱分析,2013,33(11):3124-3127. YAO Jianzhen,HAO Zhihong,TANG Ruiling,et al.Determination of high content of tin in geochemical samples by solid emission spectrometry[J].Spectroscopy and Spectral Analysis,2013,33(11):3124-3127. [8] 李小辉,孙慧莹,于亚辉,等.交流电弧发射光谱法测定地球化学样品中银硼锡[J].冶金分析,2017,37(4):16-21. LI Xiaohui,SUN Huiying,YU Yahui,et al.Determination of sliver,tin and boron in geochemical sample by alternating current(AC) arc emission spectrometry[J].Metallurgical Analysis,2017,37(4):16-21. [9] 郝志红,姚建贞,唐瑞玲,等.交流电弧直读原子发射光谱法测定地球化学样品中银、硼、锡、钼、铅的方法研究[J].地质学报,2016,90(8):2070-2082. HAO Zhihong,YAO Jianzhen,TANG Ruiling,et al.Study on the method for the determination of silver,boron,tin,molybdenum,lead in geochemical samples by ac-arc direct reading atomic emission spectroscopy[J].Acta Geologica Sinica,2016,90(8):2070-2082. [10] 郝志红,姚建贞,唐瑞玲,等.直流电弧全谱直读原子发射光谱法(DC-Arc-AES)测定地球化学样品中痕量硼、钼、银、锡、铅的方法研究[J].光谱学与光谱分析,2015,35(2):527-533. HAO Zhihong,YAO Jianzhen,TANG Ruiling,et al.Study on the method for the determination of trace boron,molybdenum,silver,tin and lead in geochemical samples by direct current arc full spectrum direct reading atomic emission spectroscopy (DC-Arc-AES)[J].Spectroscopy and Spectral Analysis,2015,35(2):527-533. [11] 贾小梅,党若凡,刘玲,等.光谱多元素分析测定的影响因素[J].广东化学,2015,42(8):185,203. JIA Xiaomei,DANG Ruofan,LIU Ling,et al.The influence factors of spectrum multi-element determination[J].Guangdong Chemical Industry,2015,42(8):185,203. [12] 彭君,仝湘滨,周林宗,等.基于深孔改进电极发射光谱法同时测定地球化学样品中微量银,锡,硼[J].中国无机分析化学,2018,8(2):3. PENG Jun,TONG Xiangbin,ZHOU Linzong,et al.Simultaneous determination of trace silver,tin and boron in geochemical samples based on deep hole improved electrode by emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(2):3.