炭酸塩融解法と酸抽出法による炭化ケイ素中不純物の誘導結合プラズマ発光分析

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タイトル別名
  • Inductively coupled plasma-emission spectrometric determination of impurities in silicon carbide by carbonate fusion and acid decomposition methods.
  • 炭酸塩融解法と酸抽出法による炭化けい素中不純物の誘導結合プラズマ発光分析
  • タンサンエン ユウカイホウ ト サン チュウシュツホウ ニ ヨル タンカ ケイ

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Impurities (18 elements) in silicon carbide powder samples were determined by inductively coupled plasma-emission spectrometry (ICP-ES). Sample solutions were obtained by either carbonate fusion or acid decomposition. In the carbonate fusion, silicon carbide (0.5 g) was fused with 2.5 g of sodium carbonate in a platinum crucible at 1000 °C for 30 min. In the acid decomposition, 0.5 g of silicon carbide was decomposed with 10 ml of hydrofluoric acid and 2 ml of nitric acid in a Teflon pressure vessel at 170 °C for 16 h. The matrix components from the carbonate fusion (about 1.1 % sodium ion and 4.5 % sulfuric acid in the sample solution) reduced the emission intensities by about 2025%. Thus, it was important to match the compositions of standard and sample solutions with regard to flux and acid. For the sample solutions obtained by the acid decomposition, the emission intensities were little affected by the matrix components (4 % hydrofluoric acid, 1.2 % nitric acid, and about 100300 μg/ml hexafluorosilicate). The detection limits for respective elements in the carbonate fusion method were higher than those in the acid decomposition method. The amounts of aluminum, boron, calcium, and chromium in silicon carbide obtained by the acid decomposition method were smaller than those obtained by the carbonate fusion method, presumably because these elements are incorporated into the silicon carbide lattice and the extraction of these elements by the acid decomposition method is incomplete. The measured values of other impurity elements agreed well between the two sample decomposition methods, indicating that these elements are segregated on the surface of silicon carbide powder particles.

収録刊行物

  • 分析化学

    分析化学 33 (11), 576-581, 1984

    公益社団法人 日本分析化学会

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