Rapid decomposition and analysis of refractory tungsten compounds by fusion with ammonium hydrogen sulfate.

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  • MATSUMOTO Ken
    Department of Chemistry, Faculty of Science, Kanazawa University
  • YUNO Mayumi
    Department of Chemistry, Faculty of Science, Kanazawa University

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Other Title
  • 硫酸水素アンモニウム融解による難溶性タングステン化合物の迅速分解と分析への応用
  • リュウサン スイソ アンモニウム ユウカイ ニヨル ナンヨウセイ タングステン

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Abstract

A simple and rapid method for the decomposition of refractory tungsten compounds has been proposed. The tungsten samples (WO3, WS2, WC, alloys and ores) were de-composed by fusion with ammonium hydrogen sulfate, which was found to be a suitably powerful flux for dissolving various refractory tungsten compounds. An accurately weighed sample (ca. 4050 mg) was placed in a dry Pyrex glass test-tube (16 mm o.d., 180 mm length). Ammonium hydrogen sulfate (ca. 2 g) was added to the tube and mixed with the sample by agitating of the tube. The bottom of the test tube was gently heated with a swirling motion over a small gas flame of a Bunsen burner with a fish-tail at a temperature of ca. 350450°C. Heating was continued until a clean, translucent yellow melt was formed. The cooled melt was dissolved in a 10% (w/v) ammonium tartrate solution. Tungsten(VI) oxide and sulfide were dissolved by heating for about 4 min, for carbide it was about 8 min. Finally, the concentration of the tungsten in the, resulting solution was determined by atomic-absorption spectrometry using a dinitrogen oxide-acetylene flame. This method was applied successfully to various hard metals and ores (scheelite). The tungsten, cobalt and iron in the samples were determined.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 46 (2), 101-105, 1997

    The Japan Society for Analytical Chemistry

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