Symposia - Symposuim on Determination of Hydrogen in Steel - Determination of Hydrogen in Steel Sampling and Analysis by Vacuum Extraction

Although hydrogen has been intensively studied in its relation to steel quality, the methods of sampling and determinations are still open to question. It is true that various procedures have been proposed but actually there has not been sufficient agreement to establish a common base from which to work. As a result, it is difficult, to say the least, to correlate the reported results of some of the investigators in this field. The present symposium, premised on methods rather than effects, should prove of considerable value. For the purpose of this discussion two methods of sampling and analysis will be considered. First, sampling of molten steel in the ingot mold by use of an evacuated tube and cylinder using conventional methods of analysis for the gases collected; second, analysis by vacuum extraction involving the use of heating equipment and the determination of the amount of hydrogen evolved from solid steel samples by measurement at reduced pressures. Both methods have been used at Duquesne Steel Works and it is believed that either may be used with considerable benefit if the limitations of each method are recognized. Evacuated Tube and Cylinder Sampling devices for gases in molten steel suggested by various investigators range from very cumbersome and complicated devices to the relatively simple evacuated tube and cylinder used by Soler for deter- mining the CO content of the bath. This latter device was adopted (Fig. I) and modified to meet conditions at Duquesne Works. The principal modifications were in placing the cylinder at the side of the tube and the use of a sleeve on the immersion end of the tube. The first modification was made so that the cylinder could be readily detached and taken to the laboratory; the second, because of the difficulty encountered in obtaining an airtight seal after sampling and because of our practice of re-using the tube. Rigid control of the method of sampling and of the handling of the sample according to plan are of primary importance in hydrogen determinations. This applies to both the sampling of molten steel and the determination of the hydrogen content of cold steel samples. Except for a few preliminary samples taken from spoons, all work on molten steels using the evacuated tube was confined to the sampling and analysis of molten steel during the pour. As mentioned, uniformity of sampling was a basic consideration. As a result, every effort was made to follow definite sampling techniques and procedures. These included control of the depth below the surface from which the sample was taken, the timing between the shutoff and taking of the sample, as well as maintenance and care of the equipment. The distance below the surface at which the sample was taken was readily controlled bv means of a crosspiece and centering device attached to the tube. The steel was poured into the mold to the hot-top junction, the tube was then lowered into the 75