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.
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