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By John A. Emery, Frank G. Snyder

Mining geology has a threefold objective: to guide prospecting for new ore, to evaluate known orebodies as development risks, and to supply the detailed knowledge of ore structures necessary for more economical extraction. The role of geology in exploration is well established. This article will deal solely with orebody evaluation and the application of geology to development and mining problems as practiced by St. Joseph Lead Co. in the southeast Missouri district, which for many years has supplied approximately 30 pct of U. S. lead production. The primary concern of the present discussion is geology in the district, not geology of the district. The southeast Missouri district, locally called the Lead Belt, includes parts of St. Francois, Madison, and Washington counties. The first recorded mining was about 1720 at Mine La Motte in Madison County on surface showings of lead ore. Later discoveries near Bonne Terre, twenty-five miles to the north, led to extensive prospecting and underground mining. To date the district has yielded well over 8 million tons of pig lead, valued at more than $1 billion. By far the greater part of the lead production has come from an area of 50 sq miles, centering Fig. 1-Central portion of southeast Missouri on the city of Flat River, as shown in Fig. 1.

Dec 1, 1956

By O. C. Wheeler

There was an increased amount of activity in the oil business in Colombia during 1934 over that of the past several years in point of production, development and exploration. The Tropical Oil Co. continued to be the only company operating on what may be called a commercial basis, although the Gulf, through its subsidiary, the Colombian Petroleum Co., was actively engaged in exploratory and developmental work on its Barco property in eastern Colombia. The Socony Vacuum interests acquired an option from Sr. Luciano Restrepo on a concession in Las Monas-Sogamoso River area and carried out geological investigations on these lands during the year. Colombian Petroleum Company The activities of the Gulf in exploration and development in Colombia during 1934 were confined to the Barco concession. The following information is furnished through the kindness of Mr. E. S. Bleecker, Chief Geologist of the South America Gulf Company. Two strings of tools were kept in operation throughout the year on the Petrolca (Tarra) structure. Three wells were completed, including one deep test, all of which were producers from one or more of the three zones which have been defined in the Lower Cretaccous limestone formation. On the Rio de Oro structure, some 45 miles northwest of Petrolea, a complete camp has been established on the Catatumbo River, about

Jan 1, 1935

George B. CoRless, Chairman. Superintendent, Gulf Coast Division, Humble Oil & Refining Co., Houston, Texas. W. H. Geis, Associate Chairman. Geologist, Los Angeles, California. Benjamin C. Craft, Secretary-Treasurer. Associate Professor, Petroleum Enginecring, Louisiana State University, Baton Rouge, La. Executire Committee George B. Corless, Chairman. M. Albertson, Production Engineer, Shell Petroleum Corporation, Houston, Texas. D. R. Knowlton, General Production Superintendent, Phillips Petroleum Co., Bartlesville, Oklahoma. R. P. McLaughlin, General Manager, Dominguez Oil Fields Co., Los Angeles, California. Hallan N. Marsh, Production Engineer, General Petroleum Corporation of California, Los Angeles, California. Theron Wasson, Chief Geologist, The Pure Oil Co., Chicago, Illinois. Production Engineering M. L. Haider, Vice-chairman. Petroleum Engineer, Carter Oil Co., Tulsa, Oklahoma. Joseph Chalmers, DeBataafsche Pet. Maatschappij, The Hague, Netherlands. Emile HugUenin, Deputy State Oil and Gas Supervisor, Los Angeles, California. Carl E. Reistle, Jr., Petroleum Engineering Department, Humble Oil & Refining Co., Houston, Texas. Production J. TERry Duce, Vice-chairman. Geologist, The Texas Company, New York, N. Y. Basil B. Zavoico, Associate Vice-chairman. Geologist, The Chase National Bank, New York, N. Y. Engineering Research R. L. Huntington, Vice-chairman. Associate Professor, Petroleum Engineering, University of Oklahoma, Norman, Oklahoma. Economics Sidney A. SwensrUd, Vice-chairman. Assistant to the President, Standard Oil Co. (Ohio), Cleveland, Ohio. Refinery Engineering Walter Miller, Vice-chairman. Vice-president, Continental Oil Co., Ponca City, Oklahoma. 10

Jan 1, 1938

By E. G. Deane

THE CHAIRMAN (P. G. BECKETT, Globe, Ariz.).-The mining of large orebodies has in the last few years been such a big factor in the copper output of this State, and, in fact, of the whole country, I feel that we should have some valuable discussion this evening on the various mining methods described in the papers which are to be read; and I hope you will start a discussion on Mr. Deane's paper. J. A. EDE, La Salle, Ill.-I would like to ask whether, the timbers being left in, they have any fires owing to that fact? E. G. DEANE.-No, we do not. The timbers in the mat seem to lose life. I cannot tell you exactly what change takes place, but they do not burn readily. There is undoubtedly a chemical change in them-a change that makes them lose all strength. I , spoke of the strength of the sills. When we first started, we put in 4 by 8 sills, but those sills had no more strength in 6 months than a 2-in. plank would have. .J. P. HODGSON, Bisbee, Ariz.- I would like to ask Mr. Deane if the central supply raise in the- center of the block has been satisfactory; and also whether in extracting the ore they put small raises up so that wheelbarrows are not used in the stope?

Jan 12, 1916

Cyanidation and Concentration of Gold and Silver Ores. By J. V. N. Dorr and Francis L. Bosqui. Second edition, completely revised. Mc-Graw-Hill Book Co., New York. $8.50.-First issued 13 years ago, this book has become a milestone in the literature of mining and metallurgy. Mr. Dorr, with the assistance of F. L. Bosqui, has completely revised the book. Its comprehensive picture of ore dressing and hydrometallurgical methods are of importance to mining engineers and operators throughout the entire field. Operating data and methods, flowsheets, testing procedures, and many miscellaneous methods of extracting bullion are given. The book is divided into two sections, the first discussing principal unit processes involved in gold and silver recovery, and the second describing with flow diagrams a number of typical treatment plants selected from the more important gold and silver mining areas in various parts of the world. International Conference on Coal Preparation in Paris. English Language edition of transactions.-The transactions of the recent conference in Paris will be presented in the form of 6 issues of the revue de l'Industrie Minerale, and may be purchased for 3000 francs per set. About 60 papers were presented at the meeting, covering a wide range of interesting subjects. Ad- dress subscriptions to: Secretariat de la Societe de l'Industrie Minerale, 19 rue du Grand-Moulin, Saint-Etienne (Loire) France.

Jan 1, 1951

THE first session of the Institute was held in the hall of the Washington University, Wednesday evening, May 27th, President Raymond in the chair. After the address of welcome by Hon. Thomas Allen, and the reply of Mr. Raymond, the following names were presented for election as members and associates, duly indorsed by the Council. They were unanimously elected : *Henry Booth, - New York City. *Charles H. Morgan, - Worcester, Mass. *Howard Painter, - West Chester, Pa. *Dr. M. J. Goodfellow, - Eberhardt, White Pine Co., Nevada *Otto Wittelshach, - Eureka, Nevada. *John T. Williams, - New York City. †Charles A. Young, - Philadelphia. *Charles E. Stafford, - Boston, Mass. *Arnold Hague, - Orange, N. J. *Richard Pearcé, - Black Hawk, Colorado. *W. R. Maffet, - Wilkes-Barre, Pa. *Prof. George A. Koenig, - University of Pa., Philadelphia *Prof. R. Nutting, Jr., - Indianapolis, Indiana. *Edwin Mickley, - Hockendauqua, Pa. *G. C. Broadhead, - St. Louis, Mo. *Dr. Adolph Schmidt, - St. Louis, Mo. *Alexander Leonhard, - St. Louis, Mo. *Edward D. Meier, - St. Louis, Mo. *John W. Meier, - St. Louis, Mo. *Prof. Forrest Shepherd, - St. Louis, Mo. *Edward Walsh, - Pilot Knob, Mo. *George Riggs, - St. Louis, Mo. †Col. Chas. B. Parsons, - Cadet, Mo. † W. A. Scott, - Mine La Motte, Mo. *Prof. Paul Schweitzer, - Columbia, Mo. *William E. Guy, - St. Louis, Mo. †William Harris, - St. Louis, Mo. *Henry Black, - Pittsburgh, Pa. †W. Noyes, - New York City. *W. Lorenz, - Philadelphia. †E. A. Whetmore, - New York City. * Members. †Associates.

Jan 1, 1875

The Sixty-fifth Congress was a "War Congress." Perhaps nothing else than war work should have been expected of it, but it had time and opportunity to do much more. Engineers have good reason for sorrow over the engineering legislation that died merely because there was no opportunity for a vote. The mineral resources of the public lands of the United States are, except the precious metals, locked away from development. For more than eight years there has been an attempt by both the executive and legislative departments of the nation to secure legislation which, under proper conditions and without detriment to the public interest, will open up these lands for development. After eight years of study, argument, conciliation, and compromise, Congress agreed in conference of the two Houses upon a measure satisfactory to it and to the Executive Department and the final draft was passed by the House of Representatives, but in the Senate it was talked to death by Senator LaFollette of Wisconsin. Some of its proponents plan to, reintroduce the bill identically as agreed to in conference into the 66th Congress, where it is hoped that by reason of its peculiar fate in the 65th Congress it will be regarded in the nature of unfinished business and thus receive early consideration and passage.

Jan 5, 1919

The American Mining Congress, of which the President is Carl Scholz, and the Secretary is J. F. Callbreath, and of which many of the officers and directors are prominent in Institute affairs, has extended to the members of the Institute a cordial invitation to attend the nineteenth Annual Session of the Congress, to be held at the La Salle Hotel, Chicago, Nov. 13 to 16, 1916, and to take part in its deliberations. The morning sessions will be, general meetings at which the attendance of all members of the Convention is hoped for, and which will he devoted to a discussion of subjects related to the three several heads, "safety," "efficiency" and "conservation." The afternoon meetings will be divided into several sections, each devoted to the discussion of subjects of interest to its special branch of the industry. It is planned to have 811 papers printed and distributed, allowing the author a limited time in which to present the salient features of his address and giving up the greater part of the time to a discussion of the subject presented by members on the floor. By this plan it is hoped to have a free expression of opinion and to provide ample time for reaching conclusions to be embodied in resolutions representing the best thought of the mining industry.

Jan 10, 1916

By R. D. Schoone, J. T. Michalak

Recovery, recrystallization, and texture development of a cold-rolled aluminum-killed steel have been studied during simulated box annealing. Two different initial conditions existed prior to cold rolling: 1) essentially all of the nitrogen in solid solution and 2) most of the nitrogen precipitated as AlN. The combined effect of nitrogen and aluminum in solid solution before annealing was to inhibit recovery and sub-grain growth at temperatures above about 1000°F and to raise the recrystallization temperature range on continuous heating at 40°F per hr from 1000"-1050°F to 1065"-1085°F. For the material with nitrogen and aluminum initially in solution there was an inhibition in the nucleation of the (001) [110] texture component and an enhancement of the (111) [110] texture component. The differences in annealing behavior mzd texture development are attributed to preprecipitation clustering of aluminum and nitrogen at subboundary sites developed by prior cold working. THE annealing of cold-worked aluminum-killed steels has been the subject of numerous investigations.'-'2 These studies have been concerned with kinetics of recrystallization, with microstructure and texture development, and with the individual and combined effects of composition, thermal history prior to cold rolling, and heating rates during subsequent annealing. It has been shown that the inhibition of recrystallization, and the development of the pancake-shaped grain and recrystallization texture characteristic of aluminum-killed steels, can be associated with the precipitation of A1N particles during a recrystallization anneal involving heating rates in the range 20" to 80°F per hr. If the AIN is precipitated before cold rolling or if more rapid heating rates are employed, the cold-rolled steels recrystallize more rapidly to an equiaxed grain structure and texture comparable to that of rimmed low-carbon steel. The retardation of recrystallization, the development of the elongated grain structure, and the pronounced (111) texture have been attributed to: 1) precipitation of A1N at prior cold-worked grain boundaries to form a mechanical barrier to grain boundary migration;' 2) precipitation on the boundaries of the growing recrystal-lizing grains as well as on cold-worked grain boundaries;'" and 3) preprecipitation clustering or precipitation on subboundaries to retard recovery, nucleation, and growth. The present study was undertaken to study in more detail recrystallization and texture development during commercial box annealing of cold-rolled aluminum-killed steels. Comparison of the annealing be- havior after cold rolling, for two different conditions prior to cold rolling, was made in an attempt to define more clearly the role of aluminum and nitrogen in forming the recrystallization texture. A) MATERIAL AND PROCEDURE The material used in this investigation was a commercial low-carbon aluminum-killed steel which was hot-rolled with a finishing temperature of about 1565"F, then coiled at about 1020°F. The composition, in wt pct, was: 0.050 C, 0.30 Mn, 0.007 P, 0.019 Si, 0.03 Cu, 0.02 Ni, 0.02 Cr, 0.045 Al, and 0.004 N. Two 4.5 by 13 by 0.078 in. sections were cut from the center section of a hot-rolled panel and one of these was reheated to provide two different conditions prior to cold rolling: low AlN: as commercially hot-rolled, with aluminum and nitrogen in solid solution; and high AlN: as commercially hot-rolled, then reheated at 1300°F for 3.5 hr to precipitate most of the nitrogen as AlN. ~etallc&a~hic examination indicated that the reheating did not change grain size nor carbide distribution (some spheroidization of pearlite was noted). Texture analysis at half-thickness level showed that both sections had the same substantially random as-hot-rolled texture. The results of check chemical analysis of each sample are given in Table I. Both sections were cold-reduced 65 pct on a laboratory rolling mill to a final thickness of 0.027 in. Cold rolling, in one direction only, was in the direction of the prior hot rolling. Specimens 1.0 by 1.25 in. were cut from the cold-rolled sheets and given a simulated box anneal in an atmosphere of 2 pct HZ-98 pct He. Specimens were heated at a constant rate of 40°F per hr from room temperature to various temperatures in the range 750" to 1300°F and cooled immediately by withdrawal to the water-cooled end of a tube furnace. The temperature in the 6-in. uniform hot zone of the furnace was controlled within 3"F. Selection of the individual specimens was made to give a random distribution of annealing temperatures with respect to location in the cold-rolled sheet. At least two specimens of each condition were annealed to the same temperature and smaller specimens for light microscopy, transmission electron microscopy, and X-ray studies were prepared from each of these. Rolling-plane sections for each of these studies were taken at half thickness. Light microscopy and transmission electron micro-

Jan 1, 1969

By R. K. McGeary, B. Lustman

The textures produced in zirconium by cold and hot rolling, and by recrystallization above and below the transformation temperature were determined. Thermal expansivities were measured in the thickness, transverse, and rolling directions of preferentially oriented zirconium and were correlated with the texture scatter in these directions. REVIOUS investigations have indicated that minor differences between hexagonal close-packed metals of similar axial ratio may appear with respect to the textures produced both on cold rolling and on subsequent recrystallization. In the case of magnesium, beryllium, and titanium, metals of axial ratio similar to that of zirconium, the ideal orientations produced by rolling are fundamentally the same, although marked variance is reported in the degree and type of scatter about the mean orientation; in those instances where recrystallization textures were observed, they were reported to be similar to the rolling textures. Measurement of the anisot-ropy of thermal expansion of both rolled and re-crystallized zirconium could not be correlated satisfactorily with the textures reported for the above metals, and therefore a study was made of the preferred orientations produced in zirconium. Reported below are the textures produced in zirconium by cold and hot rolling, and recrystallization above and below the transformation temperature, together with the results of thermal expansion measurements. Determination of Preferred Orientation Two types of zirconium were investigated: 1— "crystal bar" zirconium obtained from the Foote Mineral Co., produced by the thermal decomposition of zirconium tetraiodide, and 2—zirconium ingot obtained from the Bureau of Mines prepared by melting sponge zirconium in a graphite resistor vacuum furnace in a graphite crucible. The major impurities present in the two materials used are listed in Table I. Several of the pole figures were later checked with 0.03 pct hafnium crystal bar material and the results were identical with those to be shown for the 1.5 pct hafnium material. The materials were cold rolled to 0.014 in. in thickness as shown in Table 11. Specimens were cut from the 0.014 in. thick rolled sheets and etched to thicknesses of 0.002 to 0.010 in. Such specimens were used for exposures up to a 50' to 60" angle between the beam and plane of the specimen; for higher angles a wire shape, similar to that described by Bakarian,' was formed on an end of the original 0.014 in. sheet. A fine-bladed abrasive cut-off wheel was used to slot the sheet and to form the cylindrical cross-section. The wire shaped ends were then etched to 0.006 to 0.010 in. in diam. Although absorption of X-rays in the wire-shaped specimens does not vary with angle of rotation, the line width around the diffraction rings was not uniform, because the wire was narrower than the X-ray beam, and this condition caused some uncertainty in the estimation of azimuthal intensities. Furthermore, scanning was not practicable with this type of specimen so that spottiness of the rings due to large grain size was excessive for specimens which had been heated above about 650°C. Nevertheless, satisfactory information could be obtained for high angle exposures from the negatives by the use of both types of specimens. Transmission Laue photograms were taken using unfiltered molybdenum radiation (47.5 kv, 18 ma) and a 0.025 in. pinhole. With the film 8 cm from a 0.005 in. thick specimen exposures of about 30 min were adequate. For specimens with a coarse grain size, a device that scanned about 0.15 sq in. of sheet surface was used. An attempt was made to plot the pole figures by use of an X-ray spectrometer as described by Norton.' However, for the particular technique used, the intensity variations obtained were not considered definite enough to give reliable results, especially for the large grained recrystallized and transformed specimens. This method was therefore abandoned in favor of the standard photographic method. Nine exposures were taken of each specimen: seven exposures with the beam perpendicular to the rolling direction and at 0°, 10°, 20°, 35", 50°, 65", and 80" to the transverse direction, and two exposures with the beam perpendicular to the transverse direction and at 60" and 80" to the rolling direction. Additional exposures were then made where necessary. The intensity variations of the diffraction rings were estimated by eye. It was usually possible to estimate 3 degrees of intensity from the photograms but in some cases 2, 4, or 5 degrees were estimated. Experimental Results The preferred orientation was determined for the following treatments: 1—cold-rolled, 2—low temperature rolled, 3—cold-rolled surface layer, 4— cross-rolled, 5—hot-rolled, 6—recrystallized below the transformation temperature, and 7-—recrystallized above the transformation temperature. I—Cold-Rolled Textures: The slip plane in hexag-

Jan 1, 1952

By P. G. Shewmon, F. N. Rhines

THE determination of the self-diffusion coefficient of magnesium has been made possible recently by discovery1-1 of a radioactive isotope, Mg28 having a half-life of 21.3 hr,1 and subject to manufacture in useful quantity. In the present research this material was condensed from the vapor phase upon a surface of high purity magnesium. The progress of diffusion of the tracer atoms into polycrystalline magnesium was followed by machining layers and measuring the change in the intensity of radiation as a function of the distance of each layer from the surface. The self-diffusion coefficient was found to be 2.1 X 10-8 sq cm per sec at 627°C, 3.6 X 10-9 sq cm per sec at 551°C, and 4.4 X 10-10sq cm per sec at 468°C; the activation energy is about 32,000 cal per mol. Experimental Procedure Since there was no other published measurement of a diffusion velocity in any magnesium-base material, is was necessary to employ a number of new experimental techniques. The short half-life of Mg28 made it necessary to complete the entire experimental procedure within three or four days. This meant that the work had to be done where a cyclotron was readily accessible and that all operations, prior to the diffusion heat treatment, had to be so designed as to minimize their time requirements. Unusual problems were imposed also by the chemical reactivity of magnesium, its high vapor pressure, and the fact that no satisfactory method for elec-trodepositing magnesium on magnesium is presently available. Finally, the machining and handling of the easily air-borne radioactive-magnesium chips involved certain health hazards, resulting in the need for further experimental restrictions. Preparation of Mg28 The Mg28 was produced in the Carnegie Institute of Technology syncrocyclotron by the neutron spallation of chlorine.5 his involved bombarding a 2 gram crystal of high purity NaCl with a beam of 350 mev protons for a period of 2 hr, after which the crystal was dissolved in warm water and the Mg28 was concentrated and purified by chemical means (see Appendix). About 50 microcuries of Mg28 thus were obtained in the form of magnesium oxinate (8 hydroxyquin-olatc?), which was ignited in air to produce MgO. This in turn was reduced to magnesium metal vapor, by the method of Russell, Taylor, and Cooper," in the vacuum apparatus shown schematically in Fig. 1. Here the essential part is a tantalum ribbon, slightly dished to receive the MgO. The ribbon, pre- viously outgassed at high temperature, is heated to about 1700°C by passing an electric current through it, whereupon tantalum oxide is formed, magnesium vapor is released almost instantaneously, and condensed partly upon the diffusion sample. Diffusion-Sample Preparation: Hot-extruded magnesium rod, 21/32 in. round was used in making the diffusion specimens. The magnesium analyzed as follows: 0.004 pct Al, 0.027 pct Fe, 0.040 pct Mn, 0.0004 pct Cu, 0.0002 pct Ni, and less than 0.01 pct Ca, 0.0004 pct Pb, 0.0011 pct Si, 0.001 pct Sn, and 0.001 pct Zn. A brief study of the crystal texture of this material revealed a sharp fiber texture with the (001) plane roughly parallel to the extrusion axis. Cylindrical samples 1/2 in. long by 5/8 in. were machined from this rod, the end faces dressed on 3/0 emery, and lightly etched with 20 pct HC1 in water. These samples then were annealed for at least twice the intended time of diffusion, at the intended diffusion temperature, in order to stabilize the grain structure at about 1 mm average diameter. The annealing treatments were conducted in argon in the same apparatus and in the same manner as the subsequent diffusion treatments, which will be described presently. Thus, a strain-free plane surface was produced, but there remained a layer of MgO which had largely to be removed before the layer of Mg28 was deposited. Most of this layer was taken off by two light passes over 3/0 emery paper. The balance of the oxide and a thin layer of metal were then removed by etching 5 to 10 min in 4 pct nital (4 pct HNO3 and 96 pct ethyl alcohol) made with absolute alcohol. There followed immediately three quick rinses in: 1-49 1/2 pct methanol, 49 1/2 pct acetone, and 1 pct formic acid, 2-50 pct methanol and 50 pct acetone, and 3-pure benzene. This procedure is essentially that of Sturkey.7 The resulting surface, which was of almost elec-tropolished brightness, remained plane and was free of cold work. It could be kept clean by storing under benzene, or in a desiccator; short exposure

Jan 1, 1955

By R. D. Pehlke, J. V. Gluck, R. L. Louvet

A study has been made of the effect of small additions of bismuth on the activity of zinc in dilute solution in molten tin. Free-energy interactions have previously been determined between zinc and various third elements where the solvents were molten bismuth or molten lead.'-4 In both of these solvents, the activity of zinc exhibits a strong positive deviation from ideal behavior (at 550°C y° for zinc in lead is 11.4 and for zinc in bismuth is 3.0). The present work, using tin as the solvent, is an extension to a case where the positive deviation is considerably diminished (y°Zn at 550°C is 1.63). Several previous investigators have studied the Zn-Sn binary system; however, little data is available in the range below 0.1 mole fraction zinc.5= Previous high-temperature galvanic cell studies in the Sn-Zn-Bi ternary system included the determination by Gluck and Pehlke of interactions in the bismuth-rich corner1 and separate investigations of the central region by Oleari and Fioriani6 and by Ptak and Moser.7 Yokokowa et al.8 conducted Knudsen effusion studies in the central region; however, their experiments at 625°K were conducted somewhat below the present experimental temperature range. Their results indicated an increase in zinc activity with the addition of bismuth. The present series of experiments was conducted in galvanic cells represented as follows: Zn Zn++ in LiCI-KC1 eutectic Zn + Bi in Sn (pure reference (fused salt electrolyte) (molten alloy) standard) The experimental apparatus. a multi-electrode system employing alumina crucibles and contained in a Vycor tube under a helium atmosphere, has been described previously, as have been the experimental procedures, precautions, and the methods of data reduction.1-4,- The experimental measurements were made over the range from 450° to 650°C. Between thirty and forty measurements were made in each run. The linearity of the electromotive force vs temperature relations was verified by linear regression techniques. The correlation coefficients exceeded 0.99. The experimental results summarized in Table I include the interpolated electromotive force at 550°C and the temperature dependence of electromotive force. Only results from stable and consistent cells containing more than 0.025 mole fraction zinc are reported. Attempts to run cells at 0.01 or 0.02 mole fraction zinc were not satisfactory. This is attributed to the closeness of the free energies of formation of the chlorides of tin and zinc. Calculations employing Wagner and Werner's criteria for displacement reactions10 indicated that reduction of the zinc content to 0.01 mole fraction places the cell near the borderline concentration for a 1 pct error in measured potential. The compositions shown in Table I are the actual weighed-in amounts. Previous experience has indicated that compositional changes during the running of a stable cell are negligible.' Over the range of compositions studied for the binary alloys, the activity coefficient of zinc was essentially constant indicating that Henry's law is followed to 0.05 mole fraction zinc. The temperature, OK, de-

Jan 1, 1969

By M. T. Hepworth, A. K. Stewart

Iron containing 0.1 pct A1 and -0.9 pct P by weight was internally oxidized in the temperature range 900° to 1300° C, where the bcc structure is stabilized by phosphorous. By measuring the depth of penetration of oxygen with time in an internally oxidized zone for an imposed surface oxygen potential, oxygen permeability was determined. The dgfusion coefficient of oxygen in iron was then calculated using known solubility data, yielding the expression: where Do is the diffusion coefficient of oxygen in bcc iron in sq cm per sec and T is temperature in OK. RECENTLY Hepworth, Smith, and Turkdoganl measured the diffusivity of oxygen in bcc iron and reported the temperature dependence of diffusivity from data determined in the a, and 6 temperature ranges. Subsequently Swisher and Turkdogan' have measured the diffusivity of oxygen in fcc iron. Internal oxidation techniques were employed by these investigators and in this current study. The analysis of this technique is developed by wagner3 (presented in English by Hauffe4 and Rapp 5). In this present study bcc iron stabilized by phosphorous was used to determine oxygen diffusivity in the temperature range 900° to 1300°C. Meijerin 6 has studied oxygen permeability in this temperature range using bcc iron stabilized with 5 pct Sn. Other inves- tigators who have studied oxygen permeability in bcc iron at other temperatures are Schenck et al., 7 Bohen-kamp and Engell, 8 and Bradford. EXPERIMENTAL Electrolytic iron of 99.99 pct purity was alloyed to contain 0.897 pct P and 0.093 pct Al. The maximum weight percent phosphorous required to stabilize bcc iron between 910" and 1392°C is 0.51 pct as determined by Haughton,10 0.42 pct by Roquet and jegaden," and 0.58 pct by vogel,12 with the latter value preferred by Hansen.13 Microprobe analysis indicated that there was no segregation of the phosphorous either before or after permeability studies; therefore, the quantity of phosphorous added was assumed to be sufficient to stabilize the bcc structure. Furthermore, the permeability results of studies on this alloy agreed substantially with interpolated values from previous data on bcc iron.' An ingot of the Fe-P-A1 alloy was hot-rolled to a l-in.-thick slab. Specimens were machined to dimensions: 13/8 by $ by 1/4 in. The experimental apparatus and procedure used have been described before.' A constant oxygen potential was established by passing argon and hydrogen through a column of oxalic acid dihydrate, which has a water vapor pressure which is well-known as a function of temperature. Slab specimens were exposed to a gas mixture sufficiently lean in oxygen to prevent the formation of a surface oxide for predetermined temperature for selected times. The specimens were then quenched, sectioned, and examined metallo-graphically. All quenched specimens were iron-plated to provide protection from the outside sample edge during polishing. Fig. 1 shows a typical microstruc-ture for a specimen oxidized at 953°C for 48.00 hr at a water vapor-to-hydrogen pressure ratio of 0.20. DISCUSSION AND RESULTS The following equation was derived by Hepworth et al.' from Wagner's kinetic expressions for internal oxidation:

Jan 1, 1969

By A. J. Heckler, J. A. Peterson

A capsule technique was successfully employed to investigate the effect of nickel on the activity of nitrogen in Fe-Ni-N austenite in the temperature range 600" to 1200°C. This technique consisted of equilibrating nitrogen among various Fe-Ni alloys within a sealed silica capsule. Nitrogen transfer among the specimens occurred by N, gas at 900°, lOOO? and 1200?C. Nitrogen gas pressures within the capsules were estimated to be as high as 22 atm. The activity coefficient of nitrogen, fN , in Fe-Ni-N austenite is adequately described by the linear interaction equation: log . wt pct Ni where the standard state is chosen such that fN = I as wt pct Napproaches zero in binary Fe-N. This relationship was determined over the temperature range 873" to 1473°K and for nickel contents of 0 to 35 wt pct. ALTHOUGH chemical thermodynamics of liquid iron alloys have been extensively studied, experimental data for the solid state are needed. These thermody-namic data will provide a basis for understanding phase transformations, precipitation reactions, metal-gas equilibria, and so forth. The interaction of sub-stitutional alloying elements with the interstitial elements is of particular interest. In this investigation the thermodynamic behavior of Fe-Ni-N austenite has been studied. The solubility of nitrogen gas in iron austenite is known to obey Sieverts&apos; law up to about 65 atm.1-6 In addition, the solubility of nitrogen in Fe-Ni austenite has been investigated5"8 using the classical method of equilibrating Fe-Ni alloys with nitrogen gas at 1 atm. A capsule technique similar to that used to study the activity of carbon in alloyed austeniteg&apos;&apos;&apos; was employed in the present work to determine the effect of nickel on the activity of nitrogen in Fe-Ni austenite over the temperature range 600" to 1200°C. EXPERIMENTAL PROCEDURE A series of Fe-Ni alloys up to 35 wt pct Ni was vacuum melted and cast into 1 by 3 by 6 in. ingots. Chemical analyses at the top and bottom of each ingot demonstrated that the ingots were homogeneous with respect to nickel content. The nickel contents are given in Table I. Additional chemical analyses showed that wt pct Si < 0.05, s < 0.01, C < 0.01, Al < 0.006, 0 < 0.004, Mn < 0.002, and P < 0.002. A 2 in. section of each ingot was cold rolled to 0.015 in. The material was then decarburized to a carbon content of less than 0.004 wt pct. A portion of the material of each nickel content was nitrided to various levels in a H2-NH3 gas atmosphere to provide a source of nitrogen during subsequent equilibration. The experimental technique consisted of equilibrating the series of Fe-Ni-N alloys in a partially evacuated sealed silica capsule at the temperature of interest. Both Vycor and quartz capsules were used. In general, the final equilibrium nitrogen content for each Fe-Ni alloy was approached from both higher and lower nitrogen levels. The criterion for establishing that equilibrium was attained was that the final nitrogen content for each Fe-Ni alloy was the same irrespective of the initial level. A schematic drawing of the sample configuration in a capsule is shown in Fig. 1. The samples were arranged so that there was a minimum of physical contact. The samples were also dusted with a fine, high purity alumina powder to help prevent sticking. Several different types of furnaces were used in this study. In each case, a thermocouple was placed immediately adjacent to the capsule during equilibration and the temperature was controlled to within *4?C of that reported. At each equilibration temperature, the following times were found to be more than sufficient to attain equilibrium: 600°C-250 hr, 900°C-150 hr, 1000°C-150 hr, and 1200°C-50 hr. After equilibration the capsules were quenched in water and the nitrogen contents of the specimens determined by a Strohlein analyzer. Analyses of samples after equilibration at 1000" and 1200°C showed no silicon pickup from the silica capsules. RESULTS AND DISCUSSION Transfer Mechanism. The mechanism by which nitrogen was transferred among specimens in an initially hydrogen flushed and partially evacuated capsule equilibrated at 1000°C was investigated. After equilibration the gas in the capsule was collected over water and an estimate of the pressure at temperature

Jan 1, 1970

By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775&apos; and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,&apos; and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts&apos; gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts&apos; apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,&apos; oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen&apos; have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C&apos;." and some plastic deformation in single-crystal silicon above 900oC,&apos; the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959

By B. S. Blakeney, E. P. Abrahamson II

The effect of the transition elements in binary solid-solution additions upon the recrystallization temperature of iron has been investigated. All these elements immediately raised the temperature, the majority having their greatest effect in less than 0.10 at. pct. A correlation is noted between the rate of change of recrystallization temperature with atomic percent solute and the electron configuration of the solute element. THE work of Abrahamson and rant&apos; on binary chromium-base alloys indicated that a correspondence existed between the effect of each solute element on the brittle-to-ductile transition temperature of chromium and the ground-state electron configuration of the element added. This was felt to be a bonding phenomenon and would be expected to be observed in measurements of other properties involving the breaking or exchange of atomic bonds. From this work it was postulated that a like correspondence should be found for other properties of binary alloys, such as recrystallization. This study is an effort to check this postulation using binary solid-solution iron-base alloys. Previously, the majority of recrystallization studies were carried out on steels. However, Tammann2 investigated the recrystallization of iron as effected by Co, Ni, Si, Mn, Mo, and Cr and stated that elements with the same crystal structure at room temperature as iron appeared to be more effective in raising the recrystallization temperature. Austin, Luini, and Lindsay3 studied the effects of Ni, Cr, Mn, Co, Si, and Mo on cold rolling and annealing, but noted no trend. Abrahamson and rant,&apos; in their work on the effect of both substitutional and interstitial elements upon the brittle-to-ductile transition of chromium, have shown that the outer electron configuration in the ground state of the solute element appears to be the prime determinant of the transition temperature. PROCEDURE All alloys were made using 99.95 + pct Fe with 0.02 wt pct 0, 0.004 pct C, and 0.001 pct N. All alloying elements were 99.9 + percent pure. Metal-lographically the alloys, out to at least 0.1 at. pct, appeared to be in solid solution. Though several published phase diagrams tend to dispute this.4 All alloys were arc melted six times and cast into square 400-g ingots under an argon atmosphere.

Jan 1, 1961

For the year ending February, 1923 PRESIDENT ARTHUR S. DWIGHT, District 0 NEW YORK, N. Y. PAST PRESIDENTS HERBERT HOOVER, District 4 WASHINGTON, D. C. EDWIN LUDLOW, District 0 NEW YORK, N. Y. FIRST VICE-PRESIDENT J. V. W. REYNDERS NEW YORK, N. Y. TREASURER CHARLES F. RAND NEW YORK, N. Y. SECRETARY FREDERICK F. SHARPLESS,. . . . . NEW YORK, N. Y. ASSISTANT SECRETARY PERCY E. BARBOUR NEW YORK, N. Y.

Jan 7, 1922

By Mason K. Banks

A process has been developed which produces spodumene concentrates assaying 6.0 pct Li20 and 0.45 pct Fe203, with 70 to 75 pct recovery of spodumene. Two flotation separations are required: the simultaneous removal of mica, feldspar, and quartz as a froth product using a cationic collector, and the subsequent removal of iron-bearing minerals as a froth product while spodumene is depressed as a tailing.

Jan 2, 1953

By D. K. Crampton

THE object of this work was to obtain and correlate information on effect of internal stress in variously drawn tubes on several properties. Also, a simple approximate method of comparing types of stress distribution in such variously drawn tubes was sought. There is also included some work on comparison of single and polycrystalline materials and effect of different types of operation and preferred orientation. PREPARATION OF MATERIAL A series of tubes was drawn to study the effect of the type and degree of final reduction on various physical properties and the approximate distribution of stress intensity across the tube wall. The material used all came from a single heat of 70-30 brass melted in a regular production Ajax-Wyatt induction furnace. The analysis of the metal as cast was: copper, 70.36 per cent; lead, 0.04; iron, 0.02; zinc, balance. The material was cast in "shells" with 4 in. outside diameter and 3/4 in. wall thickness. It was drawn part way down according to the usual standard mill schedule and then by suitable individual schedules to finish by a variety of types and degrees of drawing to the same final cases in every instance; namely, 0.750 in. outside diameter by 0.080 in. wall thickness. The exact final draws, together with the percentage area reductions, diameter reductions and gage reductions are given in Table 1.

Jan 1, 1932