Analysis of single crystals of metal-borides by ICP-AES after acid-dissolution.

DOI NDL Digital Collections Web Site Web Site 4 Citations

Bibliographic Information

Other Title
  • 酸分解‐誘導結合プラズマ発光分析法による金属ほう化物単結晶の分析
  • サン ブンカイ ユウドウ ケツゴウ プラズマ ハッコウ ブンセキホウ ニ ヨル
  • 酸分解-誘導結合プラズマ発光分析法による金属ホウ化物単結晶の分析(<特集>無機材料分析のためのスペクトロメトリー)

Search this article

Abstract

A method for microanalysis of single crystals of metal-borides grown by aluminum flux method was developed by using ICP-AES. Selected single crystals (1 to 5 mg) were dissolved with a mixture of 1 ml nitric acid (1+1) and 0.05 ml sulfuric acid (1+1) in a Teflon-lined bomb by heating at 150°C for 3 h. Some borides (e.g. Ti-, Cr-, Nb- and Ta-borides) were found to be insoluble or partly soluble in the mixture. For complete dissolution of the borides, an addition of 0.2 ml hydrofluoric acid (1+1) was necessary. Tests for recovery of pure crystalline boron showed that the leakage of boron from the bomb was negligible in the presence of hydrofluoric acid. When the sample solutions containing the acid were sprayed into the ICP through a borosilicate glass sample introduction system (a nebulizer and a spray chamber), the background intensity of boron increased and seriously interfered the determination of the element. The difficulty was overcome by the use of a quartz or a commercial Teflon sample introduction system, the former system being superior to the latter both in simplicity of construction and in repeatability of measurements. Owing to the lack of certified and homogeneous standards, it was difficult to determine precision and accuracy of the method. But tentative standard deviations of boron/metal atomic ratio were obtained for TiB2 and ZrB2 as follows: B/Ti=1.92±0.04, B/Zr=1.99±0.044.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 35 (8), 646-650, 1986

    The Japan Society for Analytical Chemistry

Citations (4)*help

See more

Keywords

Details 詳細情報について

Report a problem

Back to top