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DETERMINATION OF COMBINED NITROGEN IN NIOBIUM METAL

Technical Report ·
OSTI ID:4235217
>The niohium metal is dissolved in a mixture of hot concentrated sulfuric acid, potassium sulfate, and copper sulfate. The ammonia separated by distillation from alkaline solution is determined absorptiometrically using either sodium phenale/sodium hypochlorite reagent for samples containing 5 to 90 ppm combined nitrogen, or Nessler's reagent for samples containing 90 ppm a O.44% combined nitrogen. For samples containing more than O.44% combined nitrogen, the ammonia is absorbed in standard acid, excess of which is deiermined by titration with standard alkali. The method has been used for pure niobium methl containing not less than 5 pom nor greater than 2.5% combined nitrogen. At the 5 ppm level results show a quantitative recovery with a coefficient of variation of about plus or minus 3%. At the 90 ppm level results show a negative bias of about 5% with a similar coefficient of variation ss before, and at 0.2% the results are quantitative with a coefficient of variation of about plus or minus 5%. (auth)
Research Organization:
United Kingdom Atomic Energy Authority. Industrial Group. Springfields Works, Springfields, Lancs, England
NSA Number:
NSA-13-015931
OSTI ID:
4235217
Report Number(s):
IGO-AM/S-8
Country of Publication:
Country unknown/Code not available
Language:
English