A highly sensitive spectrophotometric method for the determination of
40-400 ng of chromium(III) is described. This is based on the oxidatio
n of chromium(III) with potassium periodate in alkaline medium to form
chromate and iodate. After masking the excess periodate using ammoniu
m molybdate at pH 3, the formed iodate was treated with iodide and aci
d to generate iodine. The iodine was extracted into benzene and was st
ripped to aqueous phase by equilibrating the organic layer with sodium
sulphite solution. The stripped iodide was oxidised to iodate by brom
ine water and the excess bromine was destroyed using sulphosalicylic a
cid. The formed iodate was used to generate nitrite on treatment with
hydroxylamine. The generated nitrite was determined by diazo coupling
reaction with p-nitroaniline and NEDA. The azo dye has an absorption m
aximum at 545 nm (epsilon = 7.8 x 10(5) L mol(-1)cm(-1)) and the coeff
icient of variation is 3.2% for ten determinations of chromium at the
300 ng level. Selectivity was achieved by prior extraction of chromium
(VI) species as chromyl chloride into methyl isobutyl ketone. Chromyl
chloride tvas stripped back into sodium sulphite solution and after bo
iling off the excess SO2 with acid chromium(III), was determined.