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By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961

By M. F. Koehler

[THE LITERATURE contains relatively few thermodynamic values for interoxidic compounds, and these often are unreliable. This is especially true of data for ferrites and aluminates for which heat of formation determinations may involve extreme experimental difficulties. This report contains the results of new experimental work for obtaining the heats of formation of five ferrites (Ca2Fe2O5, CaFe2O4, MgFe2O4,, NaFeO2, and LiFeO2) and one aluminate (CaAl4O7), and a review and revision of previous similar work of this laboratory on five aluminates (Ca3A12O6,, 12/7 CaO-Al2O3, CaAl2O4, NaA1O2, and LiAlO2), The results for the 11 compounds are combined with entropy and high-temperature heat content data to derive tables of heats and free energies of formation (both from the oxides and from the elements) for the temperature range 298° 1,800° K, The relative stabilities of the compounds are discussed. The presented data all have application to ceramic reactions, and those for the calcium and sodium aluminates are applicable in considering soda-lime sintering processes for extracting alumina from silicate minerals such as day and labradorite.]

Jan 1, 1961

By Louis J. Czel

Although lithium was first discovered by Arfwedson in Sweden in 1817, it did not reach any significant status in commercial application until 1908 when Thomas A. Edison received a patent covering the use of lithium hydroxide in alkaline' storage batteries. Edison's achievement can be regarded as a major breakthrough in the development of the lithium industry. In the years prior to 1908 lithium salts had found only modest applications in the pharmaceutical and pyrotechnic fields. The next important milestone in the growth of this net industry occurred in Germany in 1918 when Metallgesellschaft at its metallurgical laboratory at Frankfort-on-Main discovered that the addition of a few hundredths percent of lithium metal to aluminum and its alloys increased-the hardness. This brought into being a new commercial use of lithium in the manufacture of bearing metals. The new material, called "Bahnmetall" (railroad, metal), was widely used for, many years in the manufacture of bearings for railroad and automotive purposes. Its use continued until the early 1930's and there was a short-lived renewal of its production during World War II. Subsequent use of-the alloy was soon outmoded.

Jan 1, 1961

By McKinnon R. L

Laboratory and field work on the use of wetting agents for suppression of colliery dust is described. Although the results were inconclusive they were not discouraging and further investigation is required. The use of certain wetting agents may constitute a healthhazard.INTRODUCTIONCoal dust presents explosion and health hazards to the coal mining industry. The problem of dust suppression is particularly acute where water alone is unsatisfactory for this purpose. The addition of a surface active agent (wetting agent) to the water should enable the dust particles to be more easily wetted and thus more easily prevented from entering and spreading through the mine atmosphere.Investigations into this effect carried out at The University of Sydney mainly under research grants from The Joint Coal Board (Dawson and Hargraves, 1955; Charlton and Curnow, 1957) are summarized, and information on the possible harmful effects of certain wetting agents is given.Twelve local manufacturers and five importers supplied 52 wetting agents in liquid, solid, powder, and paste form.The active material content varied from approximately 10 per cent to 100 per cent and the cost per pound from 8d. to 14/3.LABORATORY TESTINGPossible test methodsThree methods of laboratory testing were considered.1. The standard method for comparing wetting agents is the Draves test, used in the textile industry on cotton...

Jan 1, 1961

By T. T. Campbell

This report traces the development of techniques for the preparation of high-purity rare-earth metals. Rare-earth metals, excepting samarium, europium, and ytterbium, were prepared by converting their oxides to anhydrous chlorides or fluorides and reducing the rare-earth halides with active metals such as lithium or calcium. High-purity, anhydrous rare-earth chlorides were prepared by dissolving the rare-earth oxides in hydrochloric acid to form hydrated chlorides and by subsequently dehydrating the hydrated salts in the presence of ammonium chloride at temperatures ranging from 70° to 360° C. while under reduced pressure (50 microns to 1 inch Hg). The chlorides were also prepared by direct chlorination of rare-earth oxide-carbon mixtures. Reaction efficiencies in excess of 95 percent were obtained by either method; however, purer chlorides were prepared by the aqueous ammonium chloride conversion method. Purification of yttrium chloride by high-temperature vacuum distillation proved to be an effective method of separating, oxygen-bearing compounds from the chloride. Yttrium metal prepared from purified chloride contained significantly smaller amounts of oxygen (990 p.p.m. oxygen in yttrium metal prepared from raw chloride and 200 p.p.m. in that prepared from distilled chloride).

Jan 1, 1961

By J. I. Budnick, W. B. Ittner III, D. P. Seraphim

A reliable technique has been developed for producing single crystals of tantalum in the form of small diameter wires. By suitably heat treating these and polycrystal samples, first in an oxygen atmosphere and finally in vacuum, it has been found possible to reduce residual resistivities to 10-3 microhm-cm. The purity of these samples is thus comparable to the purities obtained in zone-refined silver, copper, and aluminum. THE growth and purification of pure single crystals of the transition metals is, in general, difficult. The high melting and annealing temperatures of these metals make it necessary to employ rather special techniques in any crystallization process. In addition, the transition metals show a great affinity for and are easily contaminated by nitrogen, oxygen, and carbon. Recently, however. a number of investigators have been successful in growing,

Jan 1, 1961

Jan 1, 1961

By E. V. Bowman

This paper is intended to deal with the material handling aspects of fine coal cleaning as applied to a recently built plaint in: southern West Virginia. This plant is processing 160 tons per hour of 1/4" x.0 coal on a two shift basis. Past experience with this very friable low volatile metallurgical coal indicated that its plastometer readings, varied directly with the size and length of time elapsing between mining' and ultimate consumption. Due to the mines location with, respect to its consumers, little could be done to decrease the time element. Studies indicated that the plastometer readings are considerably less in the minus 60 mesh range than that experienced in the plus 60 mesh sizes. Therefore, handling the coal in such a manner as to have the least amount of degradation became extremely important.

Jan 1, 1961

By W. J. Babyak, F. N. Rhines

It has long been supposed that, regardless of the mechanism by which grain boundaries increase the hardness of a ductile metal, the effect should be linearly proportional to the grain boundary area. At the present time two methods for determining grain boundary area in an isotropic aggregate are available. The first, derived by Angus and Summers,' presumes that the grain boundary area is equal to 3vn, where n is the number of grains per sq mm in a random section through the metal. This estimate is based upon the assumption that the grains are equivalent to cubes whose faces correspond with the grains as observed in the micro-section. Measurements on copper, bronze, and a brass showed that a nearly linear relation exists between 3vn and hardness. This is illustrated, for the case of brass, in Fig. 1. The second method, developed independently by Smith and Guttman2 and by Duff in, Meussner, and Rhines,3 is absolute and employs a simple linear intercept count for measuring grain boundary area. It involves no assumptions with respect to the shape and distribution of the grain boundaries. The total surface in unit volume is 2 NL , where NL is the number of intercepts between grain boundary and unit length of a test line passed randomly through the sample. In practice, NL,, the average number of grain boundaries intercepted by unit length of traverse across a prepared microsection, is ob-

Jan 1, 1961

By Richard Havens

A flotation procedure was devised by the Federal Bureau of Mines for beneficiating Mount Wheeler, Nev., beryllium ores that contain the beryllium minerals bertrandite and phenacite in a complex association with calcite, fluorspar, mica, quartz, and other accessory minerals, The method also has proven to be effective in trials on ore from the Lake George, Colo., area. Samples used in most of the research ranged from 0.49 to 0.73 percent BeO. Beryllium mineralization varied from two-thirds bertrandite to all phenacite. An unusually high grade sample containing 5 percent BeO as phenacite was floated on a batch basis to prepare concentrate for utilization studies. The beryllium minerals were floated from undeslimed pulps at natural pH using sodium fluoride and sodium hexametaphosphate (HMP), as modifiers, and a fatty acid-fuel oil combination as the collector. Key factors were the use of a minimum of about 4 pounds of sodium fluoride and between 2 and 4 pounds of HMP per ton of ore. Efficacy of the HMP was related to the grind, mineralogical composition, corollary reagents, and type and time of conditioning. Addition of the fluoride, HMP, and collector in that order, followed by appropriate conditioning after each addition, was essential for satisfactory flotation.

Jan 1, 1961

By M. J. Sinnot, J. C. Shyne

Low-frequency mechanical damping measurements were made to investigate internal friction in Fe-A1 alloys. The atomic ordering of the Fe-A1 system strongly influenced the stress-induced ordering internal friction. Magnetoelastic damping was also encounteyed and was shown to be reduced by the application of a static stress. THIS paper describes some damping experiments made on alloys of Fe and Al. Stress-induced ordering internal friction was measured with samples containing from 9.8 to 31.3 at. pct Al. Aluminum is soluble in a-Fe to about 50 at. pct and forms at least two long-range ordered structures, Fe3Al and Feu.' Stress-induced ordering internal friction is known to occur in many substitutional solid solutions, but few measurements of this damping effect have been made with alloy systems that have pronounced ordering tendencies. LeClair and Lomer developed expressions relating the relaxation strength of the damping process to the degree of atomic ordering and predicted that stress-induced ordering internal friction would be zero with complete ordering.' This concept was confirmed experimentally by Lulay and Wert using the system cd-Mg It is also consistent with the weak stress-induced ordering peaks observed in P -brass by Artman and in 16 wt pct Al Fe-Al by bert.' It was expected, therefore that the ordering characteristics of the system Fe-Al would strongly influence the stress-induced ordering internal friction exhibited by the experimental alloys. SAMPLE PREPARATION The alloys used in this investigation were induction melted under vacuum using high-purity melting stock. The iron was electrolytically refined Plastiron 101 which contained 99.85 wt pct Fe. The aluminum was a special 99.95 pct pure grade supplied by Alcoa. The only other raw material was spectrographically pure graphite which was used in small quantities as a deoxidant. The amount of carbon used was slightly in excess of the amount required to completely deoxidize the melt; this resulted in residual carbon contents of 0.01 to 0.02 pct in the finished alloys. The vacuum cast 2 1/2-in. diam ingots were hot rolled to 5/8-in. diam round bars. Portions of these bars were hot swaged and hot drawn to 0.050-in. diam wire. Straight pieces of the hot drawn wire were slowly heated to a temperature of 1300°C in a He atmosphere. After holding for 4 hr, the samples were allowed to cool in the furnace. This annealing treatment resulted in grain growth in the samples, the final grain size being about the same as the wire diameter. The grain boundaries were oriented perpendicularly to the wire axis, giving a bamboo grain structure. The existence of a preferred orientation could not be detected in these coarse grained samples. If the samples had a fiber structure, this probably would have been the same in all samples because of similar processing, thus the influence of crystal orientation on the relaxation strength would have been similar in all samples. The aluminum contents of the alloys are listed in Table I. EQUIPMENT The principle of the torsion pendulum was used for the internal friction measuring device. The

Jan 1, 1961

By N. Melnyk, H W. Habgood

The conventional low temperature process for extracting' helium from natural gas involves liquefying the whole gas stream in order to remove the relatively small fraction of helium. A process based on the selective diffusion of helium through a semi-permeable barrier is, in principle, more economical and flexible, particularly for the treatment of small re-serves and low concentrations. The well-known permeability of glass to helium offers the possibility of such a diffusion process and McAfee of the Bell telephone Laboratories showed in 1958 that practical separations could be achieved by passing natural gas over bundles of fine capillary glass tubing. Developmental studies have been carried out involving larger units and more extended field tests than those of McAfee. Fine capillary tubing of Pyrex glass 0.0035 in. diameter was prepared by drawing ordinary 6 mm. laboratory tubing in a furnace. Extraction units were pre-pared containing about 10,000 such tubes, 4 ft. long and cemented inside

Jan 1, 1961

This paper deals briefly with three of the more controversial aspects of the geology of the Mount Isa ore deposits namely the geologic structures, the method of ore deposition and the origin of the ore.In the section on geologic structures, an outline is first given of the purely tectonic deformation advocated by the early authors. The current interpretation, which differs in the proposed order of events and causal forces, is then discussed. Other concepts, which attribute all or part of the deformation to sedimentary features or preconsolidation movement, are outlined ilnd commented on.The remaining two sections deal mainly with the better known lead-zinc orebodies. In the first of these a brief description and criticism is given of the early interpretation which was based on the deposition of successive waves of mineralisation which replacedindividual beds in the shales. The current ideas, which visualise emplacement of the ore between the beds rather than replacement of them, is then discussed. The final section develops the case for a sedimentary origin of the lead-zinc ores and broadly outlines the author's ideas concerning the evolution of the Mount Isa ore deposits.INTRODUCTIONAny consideration of the geology of Mount Isa must begin with the work of Blanchard and continue with that of Hall. Individually, or as co-authors, they published various papers on the geology of Mount Isa. Of these, the best known is their "Rock Deformation and Mineralisation at Mount Isa" (1941) which gave a comprehensive account of all aspects of Mount Isa geology.It is necessary to appreciate the limits set on geological knowledge of the mine and environs in 1941 by the extent of mine development and regional geologic studies. Underground, 7 level (897 ft.) was the lowest producing level. Development on 8 (1073 ft.) and 9 (1247 ft.) levels consisted only of exploratory drives and crosscuts in the vicinity of the Davidson Shaft. The tops of the 650 and 750...

Jan 1, 1961

By P. Chiotti, G. R. Kilp

IN the study of zinc-zirconium1 and zinc-uranium2 systems, vapor-pressure measurements were made in order to establish the equilibrium phase diagrams for a pressure of 1 atm. In each of these systems, only zinc has an appreciable vapor pressure over the temperature range investigated. The zinc pressure was measured over a sufficiently wide temperature and composition range to permit calculation of the standard free energy, enthalpy, and entropy of formation for the compounds ZrZn, ZrZn2, ZrZn3, ZrZn6, ZrZn14 , and U2Zn17. In these calculations the compounds were treated as line compounds. Although the exact composition range was not determined, metallographic and thermal data indicate that the solubility range for these compounds is small. It is to be noted that the compound initially reported to correspond to the formula UZn9, 2 has been shown by the crystal structure work of Makarov and vinogradov3 to correspond to the formula U2Zn17,. The crystal structure is similar to that for the compounds Th2M17, investigated by Florio,4 et al; here M represents iron, cobalt, or nickel. Therefore, thermodynamic calculations are based on the formpla U2Zn17 EXPERIMENTAL The dew-point method employed to measure the vapor pressure of zinc over uranium-zinc alloys has been described previously.2 The same procedure and apparatus were used in measuring the zinc pressure over zinc-zirconium alloys. In the case of alloys in the two-phase region consisting of a zirconium and the compound ZrZn, the Knudsen effusion method was employed to obtain a few values in the temperature range 600" to 560°C. In most cases, tantalum crucibles were used to contain the zirconium alloys. THERMODYNAMIC PROPERTIES OFU2Zn17 A least-squares treatment of the vapor-pressure data obtained for 35 and 65 wt pct U alloys in the temperature range 650° to 940°C gave lOg10PAtm = 7,713/T + 6.33 Here, as in following equations, T represents degrees kelvin and P represents the zinc vapor pressure in atmospheres. The probable errors for the two constants were calculated to be 60.68 and 0.0563, respectively. This relation represents the equilibrium dissociation pressure for the reaction U2Zn17 (s) - 2U(s) + 17Zn(v) The solubility of zinc in solid uranium is negligible and the only additional information required to calculate the free energy of formation of U2Zn17 is the free energy of vaporization of pure zinc. K. K. Kelley5 gives the relations, AF°= 30,902 + 6.03Tlog T + 0.275 X 10-3T2 - 45.03T

Jan 1, 1961

[ARTICLE I. NAME AND OBJECT Section 1. This Society shall be known as the Society of Petroleum Engineers of the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. Section 2. The object of the Society of Petroleum Engineers shall be to furnish a medium of cooperation among those interested in the petroleum-natural gas industry an to promote the advancement of this branch of mineral technology through meetings to stimulate the preparation, reading, discussion and circulation of papers connected therewith. ARTICLE II. MEMBERS Section 1. Any person who is a member of AIME may become a member of this Society by the specified process. Section 2. Local organizations may be formed by the Society of Petroleum Engineers as subsidiary units, the membership of which shall be subject to and in accordance with the by-laws of the Institute.]

Jan 1, 1961

By H. W. Schadler

Single crystals of tungsten, which were grown by electron bombardment floating zone refining, were strained 2 pet in tension and bending at 298°, 77°, and 20°K to determine the modes and crystallography of the plastic deformation of these temperatures. At 77° and 20°K plastic deformation occurs by slip on systems of the type (011) [111] and by twinning on (112)-type planes. For crystals strained at 298°K, deformation occurs by slip in [111] directions on either (Oil)- or (112)-type planes. CURRENT models for the initiation of brittle fracture in crystalline materials are based on a knowledge of the details of their plastic deformation.1 Body-centered cubic tungsten exhibits brittle failure at temperatures below about 500 °K yet the modes and crystallography of its plastic deformation have not been studied below 1000°K. In 1924, Goucher2 reported that tungsten single crystals with a total impurity content of less than 0.01 wt pet deformed by slip on the (112) [111] system in the temperature range 1000° to 3000°K. He also observed (001) [010] slip in one crystal which was constrained by the presence of a large fissure. According to Barrett3 tungsten also deforms by twinning on the (112) plane in the [111] direction, but he gives no details on the tendency for twin formation or the temperature range in which twinning occurs. Therefore, as a necessary part of a study of the factors influencing the brittle fracture of tungsten, the modes and crystallography of the plastic deformation were determined at 298°, 77°, and 20°K. Tungsten single crystals, grown using the electron-bombardment zone-refining technique first described by Calverly,4 were deformed to between 1 and 2 pet plastic strain in tension and bending. The surface offset resulting from slip or twinning was observed with an optical microscope to determine the crystallography of the deformation. The existence of twins was proven by the standard polishing and etching technique; and the crystallography of dislocation motion was followed using the dislocation etchant described by Wolff.5 Some observations on the fracture characteristics of tungsten single crystals are included. EXPERIMENTAL TECHNIQUES Growth, Purity, and Perfection of the Crystals-Several years ago Calverly, Davis, and Lever4 dem-onstrated the feasibility of growing tungsten single crystals by the electron-bombardment floating zone-refining technique, and Carlson6 showed that crystals produced in this way had a high degree of purity and were ductile at room temperature. Tungsten single crystals produced by this technique in equipment similar to that described by Carlson were used in this study. The starting material, a powder metallurgy product, was obtained in the form of a swaged 1/8-in. rod from the General Electric Wire Plant in Cleveland, Ohio. The crystals were grown from this material in a vacuum of 10"4 mm of Hg by passing a molten zone 1/8 in. long down the rod twice at a speed of 3 mm per min. At this zone speed

Jan 1, 1961

By K. C. Dean

The combination of flotation and chemical processing methods presented in this report of the Bureau of Mines enabled treatment of typical low-grade ferberite ores from the Boulder County, Colo. area, to produce specification-grade synthetic scheelite. The overall recovery from ore to synthetic scheelite was 87 percent, based on a flotation recovery of 93 percent and a similar recovery in chemical processing. Preliminary mineral dressing studies revealed that the physical and mineralogical nature of typical ferberite ores precluded high recovery of tungsten in plus 60-percent-W03-grade products by these methods. Therefore, the flotation research was focused on attaining plus 90-percent recovery in a concentrate containing 10 percent W03. Detailed studies were made (1) to establish optimum grinding conditions for obtaining adequate mineral liberation, (2) to develop collecting and modifying reagent combinations that would enable controllable selective flotation, and (3) to define the influence of different pulp solids, temperature, pH, and time for conditioning and for the rougher and cleaner flotation stages.

Jan 1, 1961

By Ruth F. Brinkley

This circular summarizes the research and technologic activities and publications of the Federal Bureau of Mines Division of Explosives Technology4/ during fiscal year 1959 (July I) 1958-June 30, 1959). Part I briefly describes the programs that were active during the report period and presents a summary of some of the information not published elsewhere. In many instances the results are only preliminary and are subject to revision on the basis of continuing investigations. Detailed reports of all programs not security classified will be made later. Part II lists and describes briefly the publications of the Division during fiscal year 1959. If the published material has some bearing on activities still current during the report period, this is indicated by references in Part I.

Jan 1, 1961

The purpose of this talk is to report the answers to the-'two following questions: I. What unique services does the mining industry expect of mining and mineral processing engineers? II. What suggestions does industry offer to educators to help revamp curricula to meet the needs of a changing industry? As the result of many questionnaires filled out in person by presidents, managers, superintendents, chief engineers, metallurgists, and other responsible individuals in operations and management of large and small metal and nonmetallic mining companies in the U. S., and to some extent abroad, we now have some, specific answers to the above questions. Although answers to questionnaires continue to arrive at this writing (February 10) the volume already received is sufficient to clearly justify certain conclusions and observations. A copy of the tally of the first 117 questionnaires received accompanies this report, and I am certain that a compilation of additional questionnaire data will merely reinforce, the trends in thinking that have been' established thus far. Here are the results of the survey:

Jan 1, 1961

By Bee R. Waples

The Alimak Raise Method, using the Alimak Climber, has proven to be a new, fast, economical method of driving raises at the Iron King Branch of Shat-tuck Denn Mining Corporation, Humboldt, Arizona. In order to fully understand the advantages of the Alimak Raise Climber, it is necessary first to describe the basic machine; second, a complete cycle of a raise round; and third, the comparative speed and economy afforded the Iron King operation by using this new method of raise driving: The raise climber consists of a drilling platform that is raised and lowered by two 6.2 HP compressed air motors that drive, through roller chains and sprockets, three worm gears connected in series. These worm gears drive pinions which grip the guide rail rack. The worm gems are fitted with spring-loaded couplings so that a small rock or grit in the rack is passed over without disturbing the mesh between the rack and the other pinions.

Jan 1, 1961