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Chromium

Small amounts of chromium (up to 0.5 percent) may be determined colorimetrically in alkaline
solution as chromate; uranium and cerium interfere, but vanadium has little influence. The
transmittance of the solution is measured at 365-370 nm or with the aid of a filter having
maximum transmission in the violet portion of the spectrum. The standard solution used for the
preparation of the reference curve should have the same alkalinity as the sample solution, and
should preferably have the same concentration of foreign salts. Standards may be prepared from
analytical grade potassium chromate.
A more sensitive method is to employ 1,5-diphenylcarbazide CO(NH.NHC,H,),; in acid solution
(ca 0.2M), chromates give a soluble violet compound with this reagent.
Molybdenum(VI), vanadium(V), mercury, and iron interfere; permanganates, if present, may be
removed by boiling with a little ethanol. If the ratio of vanadium to chromium does not
exceed 10: 1, nearly correct results may be obtained by allowing the solution to stand for 10-
15 minutes after the addition of the reagent, since the vanadium-diphenylcarbazide colour fades
fairly rapidly. Vanadate can be separated from chromate by adding oxine to the solution and
extracting at a pH of about 4 with chloroform; chromate remains in the aqueous solution.
Vanadium as well as iron can be precipitated in acid solution with cupferron and thus separated
from chromium.
Procedure
Prepare a 0.25 per cent solution of diphenylcarbazide in 50 per cent acetone as required. The test
solution may contain from 0.2 to 0.5 part per million of chromate. To about 15 mL of this
solution add sufficient 3M sulphuric acid to make the concentration about 0.1M when
subsequently diluted to 25 mL, add 1 mL of the diphenylcarbazide reagent and make up to 25
mL with water. Match the colour produced against standards prepared from 0.0002M potassium
dichromate solution. A green filter having the transmission maximum at about 540 nm may be
used.

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