An absorptiometric rapid determination of niobium in iron and steel by the molybdenum blue method without separating it from the iron, etc., has been studied. The procedure obtained is as follows: Weigh 0.10.5 g sample to a 30 m
l platinum crucible, dissolve it with an acid mixture of 10 m
l of nitric acid and 5 m
l of hydrofluoric acid, carefully add 10 m
l of dilute sulfric acid (1+2), evaporate to fumes of sulfuric acid, allow to cool down to room temperature, and add 10 m
l of water and 5 m
l of hydrofluoric acid (1+50). Transfer the solution to a 100 m
l volumetric flask and dilute with water to the mark. Pipet a 10 m
l aliquot into a 50 m
l volumetric flask, to which add 10 m
l of water, 2.5 m
l of disodium hydrogen phosphate (0.06%), and 5 m
l of ammonium molybdate (2%) by the use of a pipet. Allow to stand for 15 minutes, add 10 m
l of dilute sulfuric acid (1+2) quickly; then, 30 seconds after the addition of dilute sulfuric acid, add 4 m
l of stannous chloride (0.5%). In measuring the 30 seconds interval, use a stop watch. Dilute immediately to the 50 m
l mark with water, measure the absorption with filter S 70. Determine the amount of niobium with the calibration curve. As the presence of more than 0.05 mg vanadium causes erratic results, follow the next procedure: Dissolve the sample with 20 m
l of aqua regia, and add 20 m
l of perchloric acid (60%); evaporate to fumes of perchloric acid. Cool, and add 200 m
l of water, 5 m
l of hydrochloric acid, 5 g of sodium sulfite anhydride, and a small amount of ashless paper pulp. Boil the solution approximately for 5 minutes to hydrolyze the niobium, etc.. Digest at 60°C about 30 minutes, filter, wash with dilute hydrochloric acid (2%) several times.
Tranfer the paper and precipitate to the platinum crucible, and ignite at a dull red heat. Treat the oxides with 10 m
l of sulfuric acid (1+2), 5m
l of nitric acid, 5 m
l of hydrofluoric acid, follow the above procedure. The time required for the analysis about was 2530 minutes.
View full abstract