Determination of zirconium by EDTA method after separation as zircon-magnesium salt

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Other Title
  • ジルコニウム-マグネシウム塩分離によるジルコニウムのEDTA定量
  • ジルコニウム-マグネシウムエン ブンリ ニ ヨル ジルコニウム ノ EDTA テイリョウ

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Description

An acidic solution containing Zr4+ was treated with a sufficient amount of EDTA (ethylenediamine tetraacetic acid disodium salt) in order to mask the other elements by their complex formation. It was treated with about 10 ml 10% H2O2 and Mg2+ in excess, stirred enough at room temperature and pH 8.8, and allowed to stand for 1015 min for the formation of precipitate. The precipitate was filtered, washed with cold water, ignited to ash, fused with KHSO4 and taken up with 100 ml H2SO4 (1:10). It was treated with 10 ml 50% ammonium acetate and EDTA of known excess, heated at pH 56 for the complex formation of Zr4+ and the amount of Zr was estimated by the back titration at pH 3 with Cu2+ using PAN (α-pyridyl-β-azonaphthol) as an indicator.<BR>In the separation method, Fe3+ was masked by EDTA and Ti4+ by H2O2. There was no interference by the presence of the other elements with the exception of Al3+ and rare earths. Since Al3+ and rare earths coprecipitated with Zr4+, it was necessary to have some of their removing operations. The back titration of Zr4+ using EDTA and Cu2+ solution was carried out successfully without influence of SO42- by the presence of ammonium acetate.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 9 (6), 503-507, 1960

    The Japan Society for Analytical Chemistry

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