Symposia - Symposuim on Determination of Hydrogen in Steel - A Modified Vacuum Extraction Apparatus

Newell1 has shown that hydrogen is removed from steel in a vacuum at a temperature of 500° to 900° C. within 136 hr. Holm and Thompson2 also state that, especially when the hydrogen is high, the results obtained by extraction at 800°C. agree with those obtained by vacuum fusion. In this laboratory, an apparatus was designed (Oct. 1940) and used wherein the piece of steel was heated at 100°F. in a Torricellian vacuum (Fig. I). This vacuum was produced by raising and lowering a "leveling bottle or bulb" containing mercury. Extensive tests were made with this apparatus. The weakness of the procedure was the possibility of leakage of air into the tube around the rubber stopper at the bottom. The present plan is to raise and lower the mercury by applying vacuum from a mechanical pump, to the top of the tube and then to a bottle of mercury in which the bottom of the tube is immersed. The Apparatus The extraction is made in a Pyrex tube A, I in. i.d. It is drawn down at the top at N and an 8-mm. i.d. tube is welded on it. To this a Pyrex stopcock E, 4-mm. bore, is welded. The tube between N and E is preferably 8 in. long and is graduated in milliliters. The total length of A to the stopcock is 28 inches. Heat is supplied by a split-tube furnace. 0 in. long by 6 in. in diameter, hinged on the side. A short pyrometer couple P is inserted through the walls of the furnace. In use this is standardized by comparison with a standard couple in a I-in. tube, just opposite this short couple. In the I-in. tube A a glass rod R, flattened at one end, supports the sample S and the length of R is so adjusted that the sample is in proper place. (It may float in the mercury.) The tube A is inserted in a large rubber stopper to fit the bottle B and extends nearly to the bottom. It is so placed that the handle of the stopcock faces the operator. In this stopper also is a short tube D bent at right angles for the application of vacuum. Also in this stopper is an 8-mm. tube C reaching nearly to the bottom; this is bent so as to miss the heater and again bent to bring it in line with and as near as possible to the upper and reduced part of tube A. On this tube C is welded a 4-mm.-bore stopcock H. In order that the two tubes may be as near as possible, the handle of stopcock H faces the back, or is the reverse of stopcock E. The total height of II above the bottom is 28 in. As explained later, this is the pressure-measuring tube C. The bottle B is about half full of mercury. The mercury must cover the ends of A and C by about I in. when they are evacuated. By tees T and rubber tubing RT the tubes A, C and D, the latter through the three-way stopcock M, are connected to the vacuum pump. A sheet of asbestos at K prevents the stopcocks E and H from becoming so hot that they leak. A good grade of vacuum lubricant prevents leakage of E and H. In order to measure the pressure of the