Gravimetric determination of silicon in octaphenyl cyclotetrasiloxane by ashing method.

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Other Title
  • 灰化重量法によるオクタフェニルシクロテトラシロキサン中のケイ素の定量
  • ハイカ ジュウリョウホウ ニ ヨル オクタフェニルシクロテトラ シロキサンチュ

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Description

Several analytical conditions were studied to determine Si in organic compounds with satisfactory precision. Octaphenyl cyclotetrasiloxane was selected as a sample because its carbon and hydrogen contents were in good agreement with the theoretical values. A mixture of 50% nitric acid and 50% sulfuric acid was the most suitable as a digestion medium. The sample sublimed without decomposition when digestion was carried out in 50% nitric acid, and the resulting value was extremely low. Using 50% sulfuric acid, the formed silicon dioxide had hygroscopic character. When the flow rate of air was too fast, silicon carbide was produced partly due to the evaporation of the digestion medium. Thus 0.2 ml/min was the recommended flow rate for the complete formation of silicon dioxide. The proposed heating program was as follows:dissolution, 200°C; wet ashing, 300330°C;dry ashing, 600°C; calcination, 950°C. The total analytical time was 40 min. The relative standard deviation was 0.0025 for this method.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 36 (6), 376-380, 1987

    The Japan Society for Analytical Chemistry

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