Determination of calcium and magnesium in silicates by batch and flow injection analyses.

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  • TAKADA Kazuya
    Department of Applied Chemistry, Nagoya Institute of Technology
  • UCHIDA Tetsuo
    Department of Applied Chemistry, Nagoya Institute of Technology

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Other Title
  • バッチ及びフローインジェクション法によるケイ酸塩中カルシウムとマグネシウムの定量
  • バッチ オヨビ フローインジェクションホウ ニ ヨル ケイ サンエン チュウ カルシウム ト マグネシウム ノ テイリョウ

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Abstract

Batch and flow injection methods were described for spectrophotometric determination of calcium and magnesium in silicates. A powdered sample of 25 mg was decomposed with hydrochloric and hydrofluoric acids at room temperature, and then diluted with water and boric acid to 50 g. The interference from iron (III) was eliminated by preliminary extraction with isopropyltropolone-benzene. Calcium was measured as a glyoxal-bis(2-hydroxyanil) complex in a 0.04 M NaOH and 25% ethanol medium, and magnesium as a Xylidyl blue II complex in a borax buffer (pH 10.4) and 50% ethanol medium containing strontium-O,O'-bis(2-aminoethyl)-ethyleneglycol-N,N,N',N'-tetraacetic acid (EGTA) and triethanolamine (TEA) for masking calcium and aluminum. On the basis of the batch method, the same three streams FIA system was constructed for both elements at the rate of 20 samples/h. The present FIA (and batch) methods gave linear working ranges of 0∼6.0 ppm (0∼1.5 ppm) CaO and 0∼3.0 ppm (0∼0.6 ppm) MgO, the detection limits of 0.03 ppm (0.01 ppm) for CaO and 0.02 ppm (0.008 ppm) for MgO and good reproducibility. The analytical results of both elements in standard rocks with the proposed methods agreed well with each other and with the certified values.<br>

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 52 (2), 115-120, 2003

    The Japan Society for Analytical Chemistry

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