R. Dass et Jr. Mehta, DITHIONITE AS A NEW REDUCTANT IN THE THIOCYANATE METHOD FOR THE SPECTROPHOTOMETRIC DETERMINATION OF MOLYBDENUM, Bulletin of the Chemical Society of Japan, 67(8), 1994, pp. 2103-2106
Sodium dithionite has been recommended as a new reductant in the thioc
yanate method for the spectrophotometric determination of molybdenum.
The study is based on prior extraction of molybdenum(VI)-thiocyanate s
pecies in ethyl acetate from 0.8 mol dm-3 HCl medium followed by reduc
tion of the complex with dithionite in the organic extract. The orange
yellow color so obtained is measured at lambda(max) 468 nm against a
reagent blank. The 1:5 (Mo:SCN) complex is stable for 1 h in ethyl ace
tate and obeys Beer's law over the concentration range 0-2.6 ppm of mo
lybdenum (optimum range for accurate determination is 0.7-2.5 ppm). Th
e molar absorptivity and Sandell sensitivity of the complex are 1.79x1
0(4) dm3 mol-1 cm-1 and 0.0053 mug Mo cm-2, respectively. The relative
standard deviation for nine replicate determinations of 2 mug Mo cm-3
is +/-1.1%. Of the tested 40 cations and 24 anions including complexi
ng agents only thiourea interferes in the procedure. The method is sen
sitive and highly selective. It is applicable to the determination of
molybdenum in steels and flue dust samples with satisfactory results.