Comparison of inert-gas-fusion and modified Kjeldahl techniques for determination of nitrogen in niobium alloys

This report compares results obtained for the determination of nitrogen in a selected group of niobium-base alloys by the inert-gas-fusion and the Kjeldahl procedures. In the inert-gas-fusion procedure the sample is heated to approximately 2700 C in a helium atmosphere in a single-use graphite crucible. A platinum flux is used to facilitate melting of the sample. The Kjeldahl method consisted of a rapid decomposition with a mixture of hydrofluoric acid, phosphoric acid, and potassium chromate; distillation in the presence of sodium hydroxide; and highly sensitive spectrophotometry with nitroprusside-catalyzed indophenol. In the 30- to 80-ppm range, the relative standard deviation was 5 to 7 percent for the inert-gas-fusion procedure and 2 to 8 percent for the Kjeldahl procedure. The agreement of the nitrogen results obtained by the two techniques is considered satisfactory