Abstract
In hydrochloric acid medium, rhenium is reduced to a lower valence using stannous chloride as a reductant. The reduced species of the metal ion forms a stable violet coloured complex with potassium ferrocyanide on heating, which can be quantitatively extracted into isoamyl alcohol and its absorbance measured. The method is free from the interference of anions like sulphate, chloride, oxalate, tartrate and EDTA. Microamounts of U(VI), Cr(VI,III), V(V), Fe(III,II), Cu(II), Co(II), Ni(II), Zn(II) and Pd(II) also do not interfere. The method has a wider Beer's law range of 0–20 μg Re/ml with a Sandell's sensitivity of 0·022 μg/cm2, and is successfully applied to the analysis of different synthetic samples containing micro amounts of rhenium where it compares favourably with the existing methods. The ratio of rhenium: ferrocyanide in the extracted species is found to be 1∶1 by Job's method of continuous variations and confirmed by the mole ratio method.
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