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Determination of traces of vanadium in molybdenum metal and compounds by ion exchange chromatography-spectrophotometry

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00142a004· OSTI ID:6114235
Down to sub-parts-per-million concentrations of vanadium have been determined in up to 5 g of molybdenum metal or 10 g of its compounds. The vanadium has been separated by cation exchange chromatography in citric acid on 3-g AG50number-X8 resin columns, followed by spectrophotometry of the 4-(2-pyridylazo)resorcinol (PAR) complex in the presence of CDTA (cyclohexanediaminetetraacetic acid) to complex possible interfering trace elements. Separations are quite satisfactory, leaving only between 5 and 30 ..mu..g of molybdenum in the vanadium fraction when 10 g of H/sub 2/MoO/sub 4/ was present originally. Recoveries of vanadium from synthetic mixtures are quantitative, and 5-..mu..g amounts of vanadium in 10 g of H/sub 2/MoO/sub 4/ have been determined with a standard deviation of 0.05 ..mu..g. Distribution coefficients of vanadium(IV) and iron(III) in citric and citric-nitric acid mixtures as well as in mixtures containing phosphoric acid are presented together with elution curves showing that even large amounts of vanadium can be retained effectively on a 3-g column. Results for the analysis of synthetic mixtures and some actual samples are included, and the influence of the concentrations of nitric, citric, and phosphoric acid on the separation is discussed.
Research Organization:
CSIR, Pretoria, South Africa
OSTI ID:
6114235
Journal Information:
Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 59:15; ISSN ANCHA
Country of Publication:
United States
Language:
English