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Jan 1, 1948

Jan 1, 1922

By T. D. Yensen, R. K. McGeary

While we have not been primarily interested in the determination of hydrogen in the alloys that we have been dealing with, we arc very glad to cooperate in this symposium on sampling and analysis for hydrogen, as we can never tell when we may find it desirable to perform such analyses. Vacuum-fusion Method Our primary interest has been oxygen and carbon, in the analysis of which we think we have become very proficient. Our oxygen-analyzing apparatus is of the vacuum-fusion type (Fig. I). This employs Dr. Derge's type of graphite cruciblc and slit sleeve, with graphite powder between, for heat insulation (Fig. 2) supported in a clear quartz bulb connected to the Pyrex glass system by means of a carefully made ground joint. The latter is kept cool by means of an air blast from a circular copper tube surrounding the joint. The crucible is heated by high-frequency induction and the 24 one-gram samples successively dropped in from the horizontal tube at the top by means of a magnet. The gases (H², CO, N2) are passed through the CuO catalyst held at 300°C. (converting CO to CO²I, H² to H²O) and the CO² and H2O frozen out in the main liquid air trap, while N2 is evacuated. At the end of the operation, shown by the termocouple vacuum gauge indicating a pressure of 10-4 mm. Hg, the analyzing system is isolated by means of the mercury cutoffs, and the CO² and H2oare determined by transferring first the CO2 and then the HzO to the small trap at the right. This is done by placing liquid air on the small trap, then removing the liquid air from the large trap for one minute, which is sufficient to evaporate the Co2 and transfer it to the small trap. The CO2 is then measured by closing the mercury cutoff at the extreme right, removing the liquid air from the small trap, warming it up to room temperature, adjusting the mercury level to one of the three marks on the glass tube (corresponding to three volumes calibrated so that I mm. Hg of CO² corresponds to 0.001, 0.002 and 0.010 mg., respectively, of oxygen) and finally reading the pressure. Liquid air is now replaced on the large trap, the mercury cutoff at the right opened, transferring the COz back to the large trap. The cutoff to the pumps is then opened, the liquid air removed for one minute, thus evacuating the CO², the pumps again cut off and the H2 O transferred to the small trap as before, except that it is now necessary to warm the large trap with a Bunsen burner in order to evaporate all the H2O. This requires about three minutes, as the inner tube must be heated to at least 100°C. In order to prevent H²O from being adsorbed on the glass walls, the glass tubing beyond the catalyst (i.e., to the right in Figs. I and 3) is kept heated to about 150°C. by means of Nichrome ribbon as shown in Fig. 3. For a I-gram sample the above amounts of oxygen (0.001, 0.002 and 0.010 mg.) 35

Jan 1, 1945

Jan 1, 1941

By Robert D. Pehlke, Weldon L. Daines

The reduction of manganese oxide from a basic slag by silicon dissolved in liquid iron at steelmaking temperatures was studied to determine the rate-controlling step for the process. The experiments were carried out under an argon atmosphere in a resistance-heated vertical-tube furnace. The two liquid phases, slag and metal, were held in zirconia crucibles. Sampling and chemical analysis of the slag phase led to time-concentration curves for the system. Results obtained by varying parameters such as temperature, stirring rate, concentration, and melt geometry defined the limiting reaction mechanism. The reduction of manganese oxide by silicon is a fast reaction and reached equilibrium within 90 min. The rate of stirring has a marked effect on the reaction rate, while, on the other hand, the effect of temperature is very small. This identifies the rate-controlling step as diffusion rather than interfaciul chemical reaction. The variation of other parameters revealed that a) diffusion of manganese in the iron phase is the slow step, b) the value of D/6 for manganese in iron at 1550°C is 7x 10-4 cm per sec, c) the energy of activation for the apparent rate constant is 7 kcal per mole, and d) increasing the amount of silicon in the iron decreases the diffusion coefficient of manganese. THE equilibrium relations pertinent to the reduction of manganese oxide from a steelmaking slag by silicon dissolved in liquid iron have been studied, but little is known about the mechanisms that control the rate of the process. The purpose of the present investigation was to study the rate of reduction by silicon and to determine the rate-limiting step. The effects of stirring rate, temperature, composition, and melt geometry were investigated as a means of identifying the controlling step. On the laboratory scale, relatively little work has been done in the area of slag-metal kinetics, primarily because of the problems confronted in attempting to contain liquid slags and metals in laboratory crucibles at steelmaking temperatures. Since graphite is an ideal material for a crucible, several investigations have been carried out on the reduction of various oxides from a slag by carbon in graphite-saturated iron and on the transfer of sulfur between a slag and graphite-saturated iron. Most of this work has been performed in induction furnaces. Studies where the container was not graphite are extremely limited. A single kinetic study of manganese transfer between molten iron and basic slags was carried out by Sano, Shiomi, and Matsushita.' These investigators prepared calcium oxide and titanium oxide crucibles to contain the two-phase system. Only a few experiments were carried out and the results had to be treated qualitatively. Despite the paucity of kinetic data, a large quantity of information is available in the literature concerning the thermodynamics2-12 and physical properties'3-21 of the slags containing manganese oxide and the dilute liquid iron alloys containing manganese and silicon which were involved in this research program. EXPERIMENTAL METHOD A vertical-tube resistance-heated furnace was used in this investigation to study the slag-metal reaction Although most previous slag-metal studies were carried out in induction furnaces, a resistance furnace has several advantages including better control of temperature and stirring rate. Hence, a resistance furnace was selected for this study, and its design is shown schematically in Fig. 1. Slip-cast, fine-grained, low-porosity, lime-stabilized cubic zirconia crucibles were used for the kinetic experiments. The crucibles were 4 1/2 in. high and 2 1/8 in. OD with a 1/16-in. wall. The crucibles were only slightly

Jan 1, 1969

Jan 1, 1942

Jan 1, 1938

Table

Jan 1, 1910

Jan 1, 1938

By P. K. Foh, C. G. Dunn

IN an investigation of the rolling and recrystalliz-ing textures obtained from single crystals of Si-Fe, Koh and Dunn included specimens in the (111) [lie] orientation.1,2 This note reports some additional results obtained on samples of this orientation set aside for further study. After, primary recrystallization longer annealing treatments at 980°C produced only normal grain growth; after 16 hr at 980°C the largest grains were approximately 0.010 to 0.020 in. in diam. The orientations of 13 of the larger grains were found by the transmission Laue method. The unidentified (110) poles of these grains have been added to the (110) pole figure obtained after primary recrystallization2 to give the plot shown in Fig. 1. When grain identifications are also included, such a plot reveals the following. Two orientations agree almost exactly with the peak pole ,density positions of component B of the primary recrystallization texture, one with component A, and one with component C. All the remaining orientations except one have (110) poles near weaker and unidentified pole density peaks. In fact, the correlation is good enough for an identification of eight components. Previously only components A, B, and C were certain. The results are perhaps even more informative when combined with the (110) pole figure of the cold-rolled crystal to give the plot shown in Fig. 2. Each of the 13 orientations is identified and uniquely determined by selecting two (110) poles per crystal, which are 90" apart. The plot shows that every grain of the 13, except grain 6, has a (110) pole in common with a (110) pole concentration of the cold-rolled crystal. The orientation relationship with the cold-rolled orientation may be expressed as approximately 25" rotations about <110> axes, which is in agreement with the results found for coarse-grained primary recrystallization.2 If primary recrystallization had occurred according to the <110> rule without preference, there would have been 12 components. Actually our limited data reveals nine of the possible 12. The integrated pole figure also shows preferences among them, since three are considerably stronger than the rest. In addition to the above direct information, the following conclusions may be drawn. Primary recrystallization of the (111) [110] cold-rolled crystal produces a limited number of weak and strong components with the larger than average primary grains from these components related to the cold-rolled crystal by 25° <110> relationships. In arriving at this conclusion of limited orientations the (111) [110] orientation has to be ruled out as a source of large primaries for two reasons. First, growth in this orientation was not observed, despite an expected high grain boundary mobility (due to its 25" <110> relationship with every component of the texture). Secondly, primary recrystallization usually produces grains in new orientations, particularly in a single orientation matrix; but (111) [110] is not new. Other orientations besides those of the <110> type may be considered unlikely, of course, because the <110> relationship holds quite well for primary recrystallization2 and should produce the large primaries. There are exceptions to this rule, but probably not enough to provide large

Jan 1, 1958

By Hon. Tasker Oddie

DURING the closing days of the last Congress a resolution was passed, creating the Senate Com-mission of Gold and Silver Inquiry. The resolu-tion charges the Commission with the responsibility to investigate and report to the Congress on Jan. 1, 1924, upon the following subjects: 1. The causes of the continuing decrease in the production of gold and silver. 2. The causes of the depressed condition of the gold and silver industry in the United States. 3. The production, reduction, refining, transportation, mar-keting, sale, and uses of gold and silver in the United States and elsewhere. 4. The effect of the decreased production of gold and silver upon commerce, industry, exchange, and prices. The personnel of the Commission is as follows: Senators Pittman, Sterling, Goodling, Walsh and Oddie. At a meeting on May 8, H. N. Lawrie, a mining engi-neer and economist, was appointed as Assistant to the Commission. The present situation with respect to the gold and silver mining industries is well illustrated by the follow-ing data: The total world production of gold (in dollars) for 1915 was $468,724,918, and for 1921, $329,915,101; as shown by the reports of the U. S. Mint; and for the year 1922, $306,793,000, which is based oh a prelimi-nary estimate; this indicates a decrease of 34.5 per cent. between 1915 and 1922. The total world production of silver (in fine ounces) for 1915 was 178,850,000 oz.; for 1921, 175,268,234 oz., a decrease of 2 per cent.

Jan 6, 1923

Jan 1, 1946