Determination of silicon dioxide in potassium-rich slate by perchloric acid dehydration gravimetric method combined with molybdenum blue spectrophotometry
WANG Lijuan1,2, YU Yahui1,2, ZHAO Tuo*1,2, WANG Dongjie1,2, XING Rongrong1,2
1. State Key Laboratory of Bayanobo Rare Earth Resources Researches and Comprehensive Utilization, Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. Ruike National Engineering Research Centre of Rare Earth Metallurgy and Function Materials Co.,Ltd., Baotou 014030, China
Abstract：Accurate determination of silicon dioxide (SiO2) in potassium-rich slate is of great significance for promoting the comprehensive development and effective utilization of silicon resources. The potassium-rich slate sample was melted and decomposed with Na2CO3-Na2O2 mixture flux at 750 ℃ to convert Si to silicate. The solution was acidified with hydrochloric acid and the silicate in sample was converted into silicic acid. After perchloric acid smoking for twice, the silicic acid was dehydrated and formed to into SiO2. The sample was filtered and rinsed. Then the filtrate and washing solution were collected into 250 mL volumetric flask. The precipitate was burned until to constant mass. Sulfuric acid and hydrofluoric acid were added to convert Si to SiF4, which was removed by volatilization. The content of SiO2 in precipitate was calculated based on the subtraction of two constant mass results. The content of SiO2 in filtrate was determined by silicon-molybdenum blue spectrophotometry at the wavelength of 785 nm. The content of SiO2 in potassium-rich slate sample could be obtained by the sum of two results above. The contents of SiO2 in potassium-rich slate samples and potassium feldspar standard substances (GBW03116) were determined for 11 times in parallel according to the experimental method. Moreover, the spiked recovery tests were also conducted by adding the standard solution of SiO2. The results showed that the relative standard deviations (RSD, n=11) were between 0.40% and 0.69%. The spiked recoveries were between 99% and 101%. The determination results of certified reference materials were basically consistent with the certified values.
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