Summary
A 2N HCl sample solution containing Mo upto 0.5 mg is boiled with hydrazine sulphate. Mo(V)-SCN complex is extracted with 1–2% TBA in chloroform from 2–3.5N HCl and 0.8–1.8M KSCN concentration. The accompanying ions are back-washed with 1 % stannous chloride solution and the color is measured at 465 nm. Beer's law is obeyed from 0–20μg Mo/ml solvent phase. Ti, V, Cr, Mn, Fe, Co, Ni, Nb, W, Re, Ru, Bi, U and Ce do not interfere in much greater amounts than in the other thiocyanate methods for molybdenum.
Zusammenfassung
Eine 2-n- salzsaure, bis zu 0,5 mg Mo enthaltende Lösung wird mit Hydrazinsulfat gekocht. Der Mo(V)-SCN-Komplex wird mit 1–2% Tribenzylamin in Chloroform aus 2- bis 3,5-n HCl und 0,8- bis 1,8-m KSCN extrahiert. Die Begleitionen werden mit 1% SnCl2 rückextrahiert und die Färbung bei 465 nm gemessen. Das Beersche Gesetz gilt bis. 20μg Mo/ml Lösung. Ti, V, Cr, Mn, Fe, Co, Ni, Nb, W, Re, Ru, Bi, U und Ce stören auch in so großen Mengen nicht, die bei anderen Thiocyanatmethoden die Mo-Bestimmung stören.
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Yatirajam, V., Ram, J. Determination of molybdenum by an improved thiocyanate method. Mikrochim Acta 62, 671–678 (1974). https://doi.org/10.1007/BF01218205
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DOI: https://doi.org/10.1007/BF01218205