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By T. E. Davidson, C. G. Homan

This report deals with a study of the effects of extreme hydrostatic pressure on a polycrystalline material which exhibits a high degree of elastic anisotropy. Metallographically prepared polycrystalline bismuth samples were subjected to pressure levels up to 20,000 atm in a piston type gas-liquid system. The observed structural changes consisted of deformation localized along the grain boundaries, which appears to be a boundary migration phenomena, and widespread slip and cross slip. Subsequent deformation is progressive with increased pressure, and is substantially different in type from the deformation characteristic of uniaxial compression. A large amount of interest has been shown in recent years in the effects of extreme pressure on metals. In this connection, many investigations into the effects of pressure on physical and mechanical properties and reactions have been undertaken. Due primarily to the experimental difficulties involved, there has not been a great deal of study of the structural changes resulting from exposure of metals to extreme pressure. It has been difficult, for instance, to produce a true hydrostatic stress state in many of the extreme pressure devices used, and also to directly examine specimens metallographically before and after pressurization. The results of a preliminary investigation into one of the effects of extreme pressure, and its associated true hydrostatic stress state, on the structure of metals are discussed herein. Metals exhibit varied degrees of anisotropy in their physical and mechanical properties. Significant among the anisotropic properties is the modulus of elasticity, which varies by a factor of as much as three in some of the fcc metals, and by much larger factors in some of the less symmetrical elements. As a result of the variation of the modulus of elasticity with crystallographic direction, shear stresses will be induced in polycrystalline samples under true hydrostatic compression. Depending on several factors, these shear stresses could become of suffi- cient magnitude to cause localized plastic deformation. Presented herein are some of the structural changes observed in polycrystalline bismuth as a result of exposure to hydrostatic pressures of up to 20,000 atm. Although several other materials in both bicrystal and polycrystalline form are also currently under investigation, bismuth was chosen initially, due to its low symmetry and moderately high degree of anisotropy in the elastic properties. The fact that extreme hydrostatic pressure can induce structural changes in some elements in the polycrystalline state is of importance in itself. However, it may also be a factor in many of the other extreme pressure effects. For instance, this localized plastic deformation could substantially lower the recrystallization temperature, thus altering the effects of extreme pressure on this phenomenon. Also, as commented on by ridgman,' the hysteresis in the polymorphic transition of polycrystalline bismuth under extreme pressures could possibly be attributed to structural changes brought about by unequal compressibility. Therefore, to accurately determine the true effects of extreme pressure on metallic substances, one first must determine if any structural changes due to hydrostatic compression are also simultaneously occurring. The purpose of this work has been to determine whether the shear stresses induced by hydrostatic pressure in an anisotropic polycrystalline material, such as bismuth, could reach a magnitude great enough to cause plastic deformation and to study the resultant structural changes and effects. THEORY In a metallic crystal, the elastic properties are dependent upon the crystallographic direction and plane. Depending upon the degree of anisotropy of the elastic properties and other factors, internal shear stresses of sufficient magnitude to cause localized plastic deformation may be induced in polycrystalline material by true hydrostatic compression. The following highly simplified two-dimensional model of two adjacent grains in a polycrystalline aggregate under hydrostatic pressure serves to schematically demonstrate how these shear stresses arise in an anisotropic material.

Jan 1, 1963

By Forrest T. Moyer

To keep the mineral and allied industries informed of trend: in the causes of accidents and to point out the need for corrective measures, the Bureau of Mines collects, analyzes, and publishes, periodically health and safety statistics. This report includes data for 1961 on injury experience, with related employment statistics, at coal mines in the United States. These data are presented in tabular form under the following headings: General Injury Experience Tables 1 to 6: Current data on number of injuries, degree of injury, frequency and severity rates, average severity, and related employment and production data by work location.

Jan 1, 1963

By B. D. Cullity, O. P. Puri

The magnetostrictia of nickel after increasing amounts of plastic elongation was measured at field strengths up to 1500 oe. In addition, the residual stress was measured by means of X-ray line shifts. The observed decrease in magnetostriction following plastic strain is shown to be associated with residual compressive stress. If a metal bar, whose longitudinal axis is taken as the x direction, is plastically elongated in the x direction and then unloaded, X-ray diffraction measurements will indicate the presence of a residual compressive macrostress 0%. However, stress measurement by means of mechanical relaxation does not reveal any macrostress. In a previous paper1 the fictitious macrostress indicated by X-rays was ascribed to a particular distribution of micro-stress, namely, one in which the bulk of the material was stressed more or less uniformly in compression and a very small portion in tension. It was shown that this distribution would account for Neurath's measurements2 of magnetic losses in silicon steel, because of the effect of residual stress on magnetostriction. The present paper is concerned directly with magnetostriction, in nickel, and with the effect on magnetostriction of the residual stress created by plastic elongation. The residual stress was determined by measurements of X-ray line shifts. MATERIAL AND METHODS Commercially pure "A" nickel was investigated. Its nominal composition, in weight percent, is 99.4 Ni + Co, 0.2 Mn, 0.15 Fe, 0.1 Cu, 0.1 C, 0.05 Si, and 0.005 S. Magnetostriction was measured by means of SR-4 electrical-resistance strain gages mounted on specimens 1/4 in. sq and 8 in. long. Magnetic fields up to about 1500 ce were provided by a multilayer, non-cooled solenoid. A considerable amount of heat was developed at the higher field strengths, and, to avoid errors due to changes in the specimen temperature, the following procedure was adopted. Each measurement of the magnetostriction X at a particular field strength H was preceded by demagnetization and an adjustment of the strain indicator to zero; the field H was then quickly switched on and the strain read immediately. Curves of ? vs H were flat for field strengths above about 750 oe for all specimens, and this constant value of X was accordingly taken as the saturation magnetostriction ?s The X-ray measurements of residual stress were made with a Norelco diffractometer on specimens cut from flat bars 1 1/4 in. wide, 1/8 in. thick, and 12 in. long. These measurements were confined to lattice planes parallel to the surface of the specimen. Two reflections were studied: the 311 CrKß line at 28 = 157 deg, and the 420 CuKal line at 28 = 155 deg. The line centers were determined by fitting a parabola to the peak of the line, as suggested by Ogilvie3 and as modified by Koistinen and Marburger.4 The CuKa doublet from the plastically elongated specimens was first resolved by the Rachinger method5. All X-ray measurements were made by counting at fixed angular positions. RESULTS The results of the magnetostriction measurements are shown in Fig. 1 and Table 1. The magnitude of

Jan 1, 1963

By J. C. Bothan

A program to provide technical in-formation on the use of fuels in pyro-metallurgical processes, from the Canadian fuel viewpoint, was initiated about five years ago by a Canadian Institute of Mining and Metallurgy liaison grou1> composed of members from the Coal Research Committee of the Coal Division and the Iron and Steel Committee of the Metallurgy Division. This paper is another of a series prepared for this program. Previous papers included a review of pyrometallurgical processes of Canadian interest, a survey of ferrous processes relevant to the development of an integrated steel industry in western Canada and a survey of the fuel requirements of the non-ferrous metals industry in Canada. It is widely recognized among per-sons familiar with the Canadian coal industry that, because of the large resources of coking coal in western Canada, the

Jan 1, 1963

By George H. Johnson

This report describes the procedures and summarizes the results of an investigation of surface subsidence above caving blocks at the San Manuel mine, San Manuel, Ariz., in order to obtain quantitative information on subsidence and ground movement caused by mining large volumes of ore. This investigation is one part of an overall study of rock mechanics being undertaken by the Bureau of Mines. Attention was given to the improvement of a rapid and precise method of surveying a large number of subsidence pins and cracks in the surface terrain. Photogrammetric methods were used as an adjunct to the triangulation subsidence surveying as well as in ordinary topographic work Maps of various kinds were prepared to show the results obtained. The computation of the survey notes was programed for an electronic digital computer at a saving of time and expense over the use of a desk calculator and trigonometric tables.

Jan 1, 1963

By Niles E. Grosvenor

Complex underground mining problems are increasing as mining depths increase. Many of these problems have been solved mainly by unsystematized trial-and-error methods based on individual experiences. This system of solving mining problems has resulted in over-cautiousness whereby a large quantity of our mineral resources are left in the ground, or not enough caution with a resultant failure of the underground opening. From studies made of physical properties of rocks, large volumes of data have been collected as a source of finding correlation among the different physical tests or among certain rock types. Most of these studies have not produced satisfactory results because the investigator usually arrives at the conclusion that the results are too scattered to be reliable. The reasons usually given as the cause of this scatter are that rocks are nonhomogenous and non-isotropic. Similar types of poor correlation that were being obtained from compression tests in the Colorado School of Mines Mining Research Laboratory led to an investigation of a good method of making a simple unidirectional compressive strength test.

Jan 1, 1963

By R. O. Dannenberg

Applicability of the fluosilicate sintering process to recovering beryllium from beryl-spodumene concentrate analyzing 1.4 to 3.7 percent BeO (10 to 30 percent beryl) was investigated. The work was one phase of a Bureau of Mines research program undertaken to assess applicability of conventional processes and to devise new procedures for treating various potential beryllium feed materials. Beryllium recovery of about 70 percent in a product of 99-percent BeO grade was achieved in treating 3D-percent beryl concentrate. The process consisted of (1) sintering a briquetted charge of concentrate, soda ash, and sodium fluosilicate for 3 hours at 750° C.; (2) extracting the soluble beryllium by multiple stages of water leaching; (3) adding caustic to the leach solution and boiling to hydrolyze and precipitate crude beryllium hydroxide; (4) dissolving the crude beryllium hydroxide in sulfuric acid and separating the solution from undissolved silica; (5) sulfidizing the acid beryllium solution to precipitate heavy metal impurities; (6) adding ammonia to the clarified sulfate solution to precipitate beryllium hydroxide; and (7) converting the hydroxide to beryllium oxide (beryllia) by calcining at 900° C. About 60 percent more sodium fluoSilicate was required per unit of beryl than is used industrially in treating 10-to 12-percent BeO concentrate (80 to 90 percent beryl). Recovery decreased, and flux requirements increased, when treating concentrates containing less beryl.

Jan 1, 1963

The dissolution of gold in cyanide has been studied, using both chemical and electrochemical techniques. The electro-chemical studies have confirmed that gold may become passive in cyanide solution if its potential becomes more positive than -O· 5 V v. saturated calomel electrode (S.C.E.). The results of the conventional solution rate tests suggest that, although the solution rate is controlled by the rate of diffusion of oxygen at low oxygen and agitation levels, when these are increased the gold may become passive and its solution rate approach a steady value, or even decrease with increasing oxygen level. The passivity of gold has been shown to be of importance in the solution of small spheres of this metal, and in the extraction of gold from a calcined auriferous pyrite concentrate.INTRODUCTIONAlthough it has been appreciated for many years (McLaurin, 1893, 1895) that dissolved oxygen is a necessary adjunct to the solution of gold by the cyanide process, attempts to quantitatively assess its effect have led to conflicting results. For example, Barsky, Swainson, and Hedley (1934) reported that an increase in oxygen concentration improved the solution rate, but Beyers (1936) claimed that such an increase would reduce the rate at which the gold dissolved.By using an electrochemical approach Kudryk and Kellogg (1954) showed that the diffusion rate of either the cyanide or the oxygen was a controlling factor, and that, if the mole ratio of cyanide to oxygen concentration was greater than 10, the solution rate was proportional to oxygen concentration.These results, although they represent some of the most careful work available, were in direct contradiction to the findings of Mills (1951), who found that gold may become passive in cyanide solution, with a resultant decrease in solution rate.

Jan 1, 1963

The Burra Burra Mine is situated in complexly folded Torrensian dolomites and limestones forming the faulted axial region of a major anticline. The orebody mined was largely of secondary origin and confined between two faults, Kingston's on the west and Tinline's on the east. The orebody occurred at the junction between cherty dolomites and a clastic limestone with a large mass of marble breccia along its western margin. Secondary ore consisted of carbonates and oxides in the breccia and the ore bed and detrital copper minerals deposited as part of a clastic breccia in sinkholes and solution cavities in the dolomites and ore beds.Primary sulphides occur disseminated in the marble breccia and in stratiform habit in the ore bed. Kingston's so-called "lode" may be mineralized marble breccia.The marble breccia appears to be of diapiric or sedimentary origin and there is evidence to support a sedimentary origin for some of the copper sulphides. No igneous rocks have been discovered within 20 miles of the mine and any hydrothermal activities were probably at comparatively low temperature. The possibility of extensive stratiform and disseminated copper sulphide mineralization in the marble breccia and ore bed requires testing by further drilling and geophysical surveys.INTRODUCTIONThe re-interpretation of Burra Burra geology and ore formation discussed in this paper resulted from a comprehensive investigation of the mine and its surrounding district begun in December 1961 and in progress at the time of writing. (February 1963). The decision to investigate Burra Burra was taken after a thorough examination of records and reports of all non-ferrous metal deposits throughout South Australia and was given impetus by a report by Thomson (1963) suggesting a sedimentary origin for the copper mineralization. Although the author does not concur fully with Thomson's interpretation there is no doubt that sedimentary processes have played an important part in the formation of the Burra Burra copper deposit, nor is there any doubt that igneous activity played no part.

Jan 1, 1963

By J. E. Hilliard

Isobaric sections of the eutectoid region of the iron-carbon phase diagram have been exgerimentally determined at 35, 50, and 65 kb. The phase boundaries were located by metallographic analysis of specimens quenched after equilibriatwn at known temperatures and pressures. With increasing pres -sure a pronounced decrease in the solubility of FesC in austenite was observed together with a depression of the eutectoid temperature. These two effects resulted in a shift of the eutectoid composition toward a lower carbon content; at 65 kb the eutectoid was at less than 0.2 wt pct C. These results are in qualitative agreement with thermodynamic calculations. It has also been shown by calculations that Fe3C in contact with saturated austenite will be stable with respect to both graphite and diamond formation at all pressures above -3.5 kb. 1 HE investigation described in this article was part of a more general study of the effect of high pressure on transformations in Fe-C alloys. Thermodynamic calculations and exploratory runs made in 1959 at the start of the program indicated an appreciable change with pressure in the phase equilibria of Fe-C alloys. However, the calculations were not considered reliable enought to provide the quantitative information required for the interpretation of the effect of pressure on the kinetics of transformations. An experimental investigation was therefore made to determine a series of isobaric sections of the eutectoid region of the phase diagram at pressures up to 65 kb. EXPERIMENTAL PROCEDURE Materials. Seven alloys with analyzed carbon contents of 0.10, 0.20, 0.38, 0.60, 0.77, 0.93, and 1.20 wt pct C were prepared from Ferrovac" iron and high-purity graphite induction melted in magnesia crucibles under argon. The ingots were hot worked and swaged down to 0.19-in.-diam rod which was then centerless ground to a final diameter of 0.125 in. Samples for chemical and spectrographic analyses were taken from each end of the rods. The prin- cipal impurities were found to be Ni, Al, Co, and Si which were present in amounts up to 0.03, 0.02, 0.01, and 0.01 wt pct, respectively. Specimens were prepared by slicing the ground rods into pills 0.06-in. thick which were silver plated to reduce decarburization during the equilibration. Silver was chosen for this purpose because of its very low solubility for carbon and its mutual immisicibility with iron. High-Pressure Apparatus. The high-pressure runs were carried out in the "Belt" apparatus.' As shown in Fig. 1, this consisted of a cylindrical cell compressed between two Carboloy punches loaded by a uniaxle press. Radial support to the cell was given by the "belt" which was a Carboloy die heavily prestressed by a series of steel binding rings. Laminated gaskets of lava and metal separated the punches from the inner surface of the "belt". A cross-section of the high-pressure cell is shown in Fig. 2. Two specimen pills were located inside a resistance heater of 0.20-in.-diam Nichrome tubing. The ends of the tube were sealed with alumina and lava pills tamped in place after the

Jan 1, 1963

By Edward M. Kawenski

Float dust deposits in return airways in bituminous coal and lignite mines present a special explosion hazard. Research is in progress at the Bureau of Mines experimental coal mine to evaluate the degree of the hazard and to develop measures for preventing dissemination of dust into the ventilating air current. To determine the extent of this hazard prevailing in operating coal mines, 711 dust samples were collected in 50 mines located in the major coal fields of the United States. The mean quantity of coal and the incombustible content of the dust in the samples were determined. The term "float dust" is used to designate particles smaller than 74 microns in diameter (particles passing a No. 200 sieve) which have settled from the air current. Dust usually found in roadways and in working places is coarser than float dust, and is termed "coarse dust" (particles passing a No. 20 sieve). Variations in amount and incombustible content of coarse dust in a midwestern mine were studied previously.

Jan 1, 1963

By R. S. McClain

Continuous-circuit flotation and batch-scale precipitation tests were made by the Bureau of Nines to determine rejection of carbon and recovery of fluorine and aluminum compounds from aluminum reduction plant residues, About 40 to 60 pounds each of aluminum fluoride and cryolite are lost for each ton of aluminum produced. Gasoline and turpentine were satisfactory for floating carbon from both fresh water and saturated solution systems. Soluble fluorine and aluminum compounds were recovered by precipitation with sodium aluminate and carbon dioxide. Over 99 percent of the carbon was removed by flotation. Fluorine and aluminum recoveries up to 77 and 63 percent, respectively, were obtained in a combined precipitate and nonfloat product, In the fresh water system the combined product was mostly cryolite with some gibbsite. In the saturated solution system the product was mostly sodium fluoride, some cryolite, and minor amounts of gibbsite.

Jan 1, 1963

By d&apos, Kathleen J. Amico

THIS SUMMARY appears in Minerals Yearbook volumes I and III, which cover mineral production in the United States, its island possessions, the Canal Zone, and the Commonwealth of Puerto Rico, as well as the principal minerals imported into and exported from the United States. The several commodity and area chapters contain further details on production. A summary table comparing world and U.S. mineral production also is included. Mineral production may be measured at any of several stages of extraction and processing. The stage of measurement used in the chapter is normally what is termed "mine output." It usually refers to minerals in the form in which they are first extracted from the ground, but customarily includes for some minerals the product of auxiliary processing operatons at or near mines.

Jan 1, 1963

By D. J. Bauer

Solvent extraction techniques were used to determine the extraction sequence of yttrium and the rare-earth elements in an amine solvent extraction system. Single-stage extraction with Primene 81-R resulted in separation factors of 3.8 between yttrium and dysprosium and 25 between yttrium and cerium. Yttrium was concentrated in the aqueous phase. EDTA and DTPA, as aqueous phase counterextractants, enhance separation factors in mine-rare-earth sulfate systems. Yttrium separation from heavy rare-earth elements exhibits marked sensitivity to the position of yttrium in the selectivity scale of the rare-earth elements with the sequestrants. Yttrium-ytterbium separation is more effective with EDTA, whereas yttrium-dysprosium separation is more effectively increased with DTPA.

Jan 1, 1963

Flat jack stress determinations in selected colliery roadways have revealed a range of measured stress from 330-p.s.i. tension to 3,750 p.s.i. compression. Photoelastic examination of loaded plastic and actual rock mo.odel mine openings has shown that the primary horizontal stress required to attain these measured stresses would be from one to three times the superincumbent vertical load.Examination of roof movement with a. borehole oxtensumeter and a series of anchors at various horizons to 30 feet in a. vertical roof borehole showed that when a standing face waa.s advanced the roofmovement was practically confined to the lower two feet. The ma.j ority of this movement occurred during the 36 hours after mining at this face commenced.The use of a. radioactive isotope and a. scintillation counter in a. pair of parallel bcreholes promises to be sensitive and accurate method of roof bedding plane crack detection.

Jan 1, 1963

By W. L. Anderson

Standard tellurium analytical procedures were modified to obtain the greater sensitivity needed to support a survey of tellurium resources by the Bureau of Mines. Resulting volumetric and spectrophotometric methods for determining tellurium in all types of tellurium-containing materials are described. Sample decomposition and preliminary separations of interfering selenium, gold, and silver are the same in both procedures. The volumetric method is applicable to samples containing a minimum of 10 parts per million of tellurium, In this method the tellurium is reduced to elemental form, and the colloidal suspension is titrated with 0.01 normal iodine solution. The weight of sample for analysis, from 0.25 to 10 grams, should be selected so that the sample contains 0.1 to 5 milligrams of tellurium. To insure accuracy, duplicate samples should be run and the results averaged, particularly on samples of low tellurium content: The limit of determination is 0,001 percent tellurium, which is equivalent to 0.1 milligram of tellurium when using a 10-gram sample. The spectrophotometric method is particularly applicable to low-tenor materials containing from 0.5 to 50 parts per million of tellurium. Up to 10 gram samples are required for making accurate determinations in the low-concentration range. The sample used should contain between 5 and 100 micrograms of tellurium. The turbidity of a colloidal suspension of tellurium prepared from such a sample is determined in a spectrophotometer .t at a. wave-length of 440 millimicrons, and this value is compared with those of standard samples containing known amounts of tellurium.

Jan 1, 1963

By L. H. Adami

This paper reports the results of solution calorimetry conducted to obtain the heats of formation of crystalline FeS04?6.952H20 and FeS04?1.008H20, from. which values were derived for the stoichiometric compounds FeS04?H20 and FeS04?H20. Also included are derived values of the free energies of formation and dehydration. This work was undertaken primarily to fill a need for data for pure, easily obtainable ferrous compounds that are suitable for use as calorimetric intermediates, The ferrous sulfate hydrates meet the essential requirements for this use.

Jan 1, 1963

By C. W. Spencer, J. T. Smith

GRAIN-BOUNDARY surfaces are penetrated by a liquid phase when the liquid-solid interfacial tension is less than one-half the tension of the grain-boundary surfaces. Grain growth may occur in the presence of this liquid phase. burke1 reports that grain growth of this nature has been observed in two-phase ceramic systems. He suggests that the presence of a grain-boundary liquid may accelerate or decelerate the

Jan 1, 1963

By C. W. Grate

Cooperative Education is by no means a new idea. The first such program was instituted at the University of Cincinnati in 1906 by the late Dean Herman Schneider with twenty-seven engineering students participating. Today, more than fifty years later, there are in excess of one hundred institutions' with some such program in which thousands of students, are participating in the fields of Liberal Arts, Engineering, and Business Administration. At the same time, according to a conclusion reached during a study of work-study college programs, copyrighted in 1961 by Thomas Alva Edison Foundation, and from which we quote; "We were amazed at the lack of-information about cooperative education among school and college staffs and students, among parents and employers, and on the part of the public generally."

Jan 1, 1963

By H. A. Hancock, L. M. Pidgeon

Equilibrium carbon monoxide pressures were measured over the reaction between chromium oxide and a number of solid ferrochromium alloys in the composition range 0.4 to 4.8 pct C and 0 to 49 pct Fe. Measurements were also made for the carbides Cr23C6 and Cr7C3 which agreed well with previous investigations. Between 1050°and 1400°C the pvessures varied from 0.1 to 56 mm and increased markedly with the iron and carbon contents of the alloys. The data were used to estimate the activity of carbon in the alloys and to calculate the equilibrium conditions for the decarburization of a useful range of ferrochromium alloys. WHEN ferrochromium is produced by the reduction of chromite with carbon in an electric arc furnace it invariably contains up to 10 wt pct C. For many purposes such as the production of stainless steel, it is necessary that the carbon content be as low as from 0.02 to 0.05 pct. Thus an important part of the ferrochromium industry consists of the production of low carbon ferrochromium. The classical Bessemer steelmaking technique cannot be used to oxidize low carbon contents in chromium and ferrochromium alloys without also oxidizing the chromium. Recently a new commercial process2-4 has been introduced for oxidizing carbon from high chromium content alloys which consists of heating the solid alloy with such oxidizing agents as Cr2O3, Fe2O3, or SiO2 in a retort at reduced pressures. By maintaining the carbon monoxide pressure below the equilibrium value for the system, the carbon can be removed as carbon monoxide without oxidizing the chromium. The equilibrium conditions for the decarburization of solid chromium carbon alloys have been determined by Boericke5 who measured the carbon monoxide pressure over the reaction between the various chromium carbides and chromium oxide. A typical reaction is shown below. Cr23C6 + 2Cr2O3 =u 27Cr + 6CO [1] These values are not applicable to the decarburization of commercial ferrochromium alloys which invariably contain major amounts of iron. The present investigation was therefore undertaken to measure the change in the equilibrium carbon monoxide pressure brought about by additions of iron to the Cr-C-0 system, thus extending the work of Boericke into the region of the production of low carbon ferrochromium. MATERIALS AND METHOD Materials. Measurements were made on two carbides of chromium, Cr233C6 and Cr7C3, and fifteen Fe-Cr-C alloys. The chromium carbides were made

Jan 1, 1963