Determination of trace silicon in high-purity germanium dioxide by inductively coupled plasma atomic emission spectrometry after matrix separation
The purity of high purity germanium dioxide directly affects the quality of optical fiber germani-um tetrachloride and zone-refined germanium ingot.According to the non-ferrous metal industry standard YS/T 37.2-2018,the high purity germanium dioxide sample is placed in a platinum-gold crucible and di-gested in a closed evaporator,and then transferred to a dust-proof glove box for the determination of sili-con content by molybdenum blue spectrophotometry.However,this method has long process and compli-cated operation.In this paper,the high purity germanium dioxide sample was placed in a polytetrafluoro-ethylene beaker in ultra-clean laboratory.After complete dissolution with 12 mL of hydrochloric acid at 120 ℃,the solution was continuously heated until the matrix was evaporated and removed in the form of germanium tetrachloride.In this process,the silicon impurities were enriched in the sample solution.Then the silicon content was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).A method for the determination of trace silicon in high-purity germanium dioxide by ICP-AES after matrix separation was established.The linear range of the calibration curve was 0.02-0.20 pg/mL with the correlation coefficient of 0.999 1.The limit of detection of silicon in this method was 0.016 μg/g.The contents of trace silicon in three high-purity germanium dioxide samples were determined according to the experimental method.The relative standard deviations(RSD,n=7)of the determination results were less than 6％,and the spiked recoveries were between 91％and 102％.
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