THE DETERMINATION OF COMBINED NITROGEN IN BERYLLIUM METAL
The sample is dissolved in dilute sulfuric acid whereby the combined nitrogen is converted to ammonium sulfate. Ammonia liberated from the solution by addition of excess sodium hydroxide solution is separated by steam distillation. The ammonia in the distillate is determined absorptiometrically using sodium phenate/sodium hyppchlorite reagent, Nessler's reagent, or by titration depending on the level of combined nitrogen in the sample. (auth) l5935 The sample is dissolved in nitric and hydrochloric acids and diluted to standard volume. An aliquot is heated to fuming, with sulfuric acid, to remove nitrate, and then diluted to a known volume. An aliquot of this solution is made strongly acid with hydrochloric acid and the molybdenum determined absorptiometrically as the dithiol (4-methyl-1: 2-dimercapto benzene) complex which is maintained in homogeneous solution by the addition of n-butyl alcohol. (auth) l5936 The vanadium is determined absorptiometrically as the peroxy- vanadium complex without prior separation from the uranium, An aliquot of a nitric acid solution of the alloy is evaporated to dryness and the residue vanadium is first oxidized with potassiunm permanganate and then with hydrogen peroxide and the absorbancy measured at 5200 A after standing in the dark for an hour. The method is applicable to the determinision of vanadium within the range 0.05 to 0.30% in uranium-vanadium alloys. Up to at least 0.2% of iron and 0.4% of molyblenum do not interfere, but chromium does interfere above 0.01%, (auth) l5937 A portion of the metal in the form of turnings or powder is dissolved in a mixture of nitric and hydrochloric acids, filtered and the insoluble portion treated ution is added to a mixture of hydrochloric acid and ammonium molybdate. molybdate complex, oxalic acid is added to decompose phospho and arseno- molgbdates and sodium sulfite to prevent fading of the ''molybdenum blue.'' An excess of sulfuric acid is added to prevent reduction of the molybdic acid and the silicon determined absorptiometrically, after reduction of the complexed molpbdenum with stannous chloride. The insoluble residue is fused with sodium hydrxide and after adjusting the acidity, the silicon content is determined by a similar method to that used for the uranic solution. (auth)
- Research Organization:
- United Kingdom Atomic Energy Authority. Industrial Group. Springfields Works, Springfields, Lancs, England
- NSA Number:
- NSA-13-015934
- OSTI ID:
- 4235095
- Report Number(s):
- IGO-AM/S-41
- Resource Relation:
- Other Information: Orig. Receipt Date: 31-DEC-59
- Country of Publication:
- Country unknown/Code not available
- Language:
- English
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