Fundamental Studies on Analysis of Silicate Anions using Improved Trimethylsilylation Method

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The improved trimethylsilylation method reported previously is used in order to determine silicate anions present in various crystalline silicates and to measure the variation in the distribution of silicate anions in silicates during crystallization of glassy samples in CaO–50 mol%SiO2, CaO–43.3 mol%SiO2 and PbO–33.3 mol%SiO2.<BR>Results of these experiments are summarized as follows:<BR>(1) The orthsilicate crystal such as 2SrO·SiO2, 2CaO·SiO2 and 2ZnO·SiO2, and the pyrosilicate crystal such as 3CaO·2SiO2 are determined to be mainly composed of SiO44− and Si2O76− respectively, while the Li2O·SiO2 crystal is considered to comprise infinite chains, because the trimethylsilyl derivative is not detected gas-chromatographically.<BR>(2) On crystallization of glassy samples in CaO–50 mol%SiO2 and CaO–43.3 mol%SiO2, types of silicate anion determined by this method are in good agreement with those analyzed on the base of IR and X-ray powder data.<BR>(3) On crystallization of glassy PbO–33.3 mol%SiO2, different temperatures of heat treatment for crystallization result in the presence of different types of silicate anions. This observation suggests the presence of various compounds of 2PbO·SiO2 as shown previously by Götz.<BR>On the basis of the above result, it is concluded that this method is useful for the analysis of silicate anions in synthetic silicate crystals and glasses.

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