TITRIMETRIC DETERMINATION OF ZIRCONIUM. I. TITRATION OF ZIRCONIUM WITH POTASSIUM PERMANGANATE IN AN ALKALINE MEDIUM
The possibility of an indirect determination of Zr by an oxidation- reduction titration of mandelic acid with KMnO/sub 4/ solution was studied. As a preliminary step the method of titrating mandelic acid and p- bromomandelic acid with KMnO/sub 4/ solution in an alkaline medium (l to 2N NaOH) was worked out; Nb/ sub 2/O/sub 5/, Ta/sub 2/O/sub 5/, SiC/sub 2/, and WO/sub 3/ did not interfere. The compounds were quantitatively oxidized in the titration to benzoic and p- bromobenzoic acid. Approximately 11% more than the theoretical amount of KMnO/ sub 4/ was used up, apparently because of auto-decomposition. The precipitation of Zr with mandelic acid took place quantitatively, and the precipitate formed had a stoichiometric composition. In the determination of Zr, the solution to be analyzed, which contained 2 to 20 mg Zr was evaporated to 20 to 100 ml; fifteen to eighty milliliters concentrated HC1 was added, the solution was heated to 95 deg , fifteen to eighty milliliters concentrated 16% solution of mandelic acid was added dropwise while stirring, and the mixture was kept on a water bath for several hours. After 1 to 2 days the precipitate was filtered off using a glass filter, washed first with mother liquor, then with ethanol and ether, dried at 110 to 120 deg , and dissolved in 5 to 6N Na/sub 2/CO/sub 3/ (4 portions of 5 ml each) on the filter while applying suction. To the resulting solution 10 ml of 23% NaOH solution and 20 ml 0.5N KMnO/sub 4/ were added. The solution was allowed to stand for 10 rain, acidified with an H/sub 2/SO/sub 4/ solution, and, on adding 20 ml 0.5N H/sub 2/C/sub 2/O/sub 4/, heated to 60 deg and titrated with 0.1N KMnO/su b 4/ solution. A control experiment was conducted simultaneously. 1 ml 0.1N KMnO/sub 4/ corresponded to 0.5136 mg Zr. The error was plus or minus l%.
- Research Organization:
- Originating Research Org. not identified
- NSA Number:
- NSA-14-022871
- OSTI ID:
- 4166004
- Journal Information:
- Magyar Kem. Folyoirat, Journal Name: Magyar Kem. Folyoirat Vol. Vol: 65, No. 1
- Country of Publication:
- Country unknown/Code not available
- Language:
- English
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Related Subjects
CHEMICAL REACTIONS
CHEMISTRY
DECOMPOSITION
ERRORS
ETHANOL
ETHERS
FILTERS
MANDELIC ACID
MANGANESE COMPOUNDS
MANGANESE OXIDES
NIOBIUM OXIDES
ORGANIC ACIDS
ORGANIC BROMINE COMPOUNDS
OXIDATION
PERMANGANATES
POTASSIUM COMPOUNDS
PRECIPITATION
QUALITATIVE ANALYSIS
QUANTITATIVE ANALYSIS
REDUCTION
SILICON OXIDES
SODIUM HYDROXIDES
SOLUTIONS
SULFURIC ACID
TANTALUM OXIDES
TUNGSTEN OXIDES
ZIRCONIUM