モリブデンの新キレート滴定法
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概要
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When molybdenum (VI) is treated with hydrazine sulfate, the reduced molybdenum (V) reacts with EDTA forming a complex with 2: 1 mole ratio of Mo/Y, and the complex can be used for the complexometric titration of molybdenum. But another EDTA complex is formed with molybdenum reduced by hydroxylamine hydrochloride.<BR>The two molybdenum (V)-EDTA complexes were compared spectrophotometrically. For the EDTA complex of molybdenum (V) reduced by hydroxylamine, the molar ratio method as well as Jobb's method of continuous variations gave the same mole ratio of Mo/Y 1 : 1.<BR>Molybdenum (V) reduced by hydroxylamine reacted stoichiometrically with EDTA over the pH range of 05, and the complex was applicable to the complexometric titration of molybdenum.<BR>To a sample solution containing 10 to 30 mg of molybdenum, add an aliquot of 0.01<I>M</I> EDTA solution and adjust the pH to about 2. Boil for 10 to 15 minutes. After cooling, titrate with 0.01<I>M</I> bismuth solution with xylenol orange as an indicator, or alternatively titrate with 0.01<I>M</I> copper solution at pH 4.5 with PAN as an indicator.<BR>The method was applied to the analysis of ferromolybdenum with satisfactory result.
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