Papers - Fractional Vacuum-fusion Analysis for Determination of Oxygen in Steel (With Discussion)

About three years ago eight standard steels were prepared for the cooperative investigation of methods for oxygen analysis, sponsored by the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers and by the National Bureau of Standards. A preliminary report of the results was made at the annual meeting of the A.I.M.E. in February, 1936. † This report showed the reliability of vacuum-fusion methods and further brought out certain advantages of the fractional vacuum-fusion method. The results obtained by the authors with the latter method will be discussed here, with some comments on the procedure for those who are interested in determinations of gases in steel. Some additional comments are offered on the use of the polarizing microscope for identifying the inclusions in the steel to check and amplify the findings of the fractional vacuum-fusion analysis. For details of the fractional method, see the paper by L. Reeve1. Degassing the Crucible One of the sources of error in vacuum-fusion methods has been the blank gases evolved from the graphite crucible after preliminary out-gassing. We have used 1750" C. as the outgassing temperature. This gives a base pressure at that temperature of less than 0.030 mm. after one hour and of 0.004 mm. on dropping the temperature to 1575" C. At lower extraction temperatures the base pressure is 0.001 mm. at 1050" C., 0.002 mm. at 1170" and 0.003 mm. at 1320' C. Because of the size of our induction coil we are limited to this temperature, although it 'would be advantageous to use 1950" to 2000" C. Hamilton2, after outgassing at 1850" C. for 100 min., was able to reach a base pressure of 0.001 mm. for a temperature of 1700' to 1725" C. This would give a blank corresponding to less than 0.00015 per cent 02 and 0.00005 per cent H2. Chipman and Marshall outgas at 2000" C. for one hour by using a special construction