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By Milton E. Wadsworth, John N. Ong, W. Martin Fassell

The temperature and oxygen concentration dependence on the reaction of sphalerite in oxygen at pressures from 6 to 640 mm Hg have been investigated in the temperature range 700° to 870°C. Sphalerite has been found to oxidize linearly over this entire temperature and pressure range. At higher rates, considerable self-heating was observed. The dependence of the oxidation rate on the oxygen concentration may be expressed by: Rate = k' where k' is the specific rate constant and 0 = K1[O2]/(1 + KI[O2]), where K1 is the equilibrium rate constant for the adsorption of oxygen on sphalerite. Values of the activation energy and the enthalpy of adsorption were found to be 60.3 and —59.6 kcal per mol, respectively. Data have been presented that indicate conditions under which either a sulphatizing or an oxidizing roast may be obtained. ROASTING processes have been employed in the metallurgy of a great number of basic metals in use today. Until recently, however, little attempt has been made to deduce the fundamental mechanism by which oxidation takes place. Structural changes upon oxidation have been investigated1 = and thorough work has been performed with regard to the reaction products and the thermodynamics of the oxidation reactions. The objective of this investigation was to determine the rate of oxidation of sphalerite and to apply the absolute reaction rate theory in the theoretilcal interpretation of the experimental results." "O Description of Apparatus The apparatus contains the following features: 1—a furnace with gas system, 2—an autographic weighing system, and 3—a temperature control system. Furnace With Gas System—The furnace was mounted by a yoke on each end and was free to travel up and down on steel guide rods, permitting the introduction and removal of samples from the apparatus with minimum difficulty. The furnace was heated by three sections of Kanthal wire wound externally on a zirconia tube and insulated with Fiber-frax. Pure gases or mixtures of gases were introduced into the lower end of the furnace through two flowmeters, a mixing chamber, and a gas-tight sparger, Fig. 1. The gaseous products of the reaction and the unused gases were prevented from escaping to the atmosphere by maintaining a small negative pressure on the system. This procedure permitted air from the outside to enter through the small an-nulus around the quartz suspension fiber and prevented the escape of the internal gases. Autographic Weighing System—The autographic weighing system consisted of an adapted gold balance, a photoelectric circuit, and a weight recorder, Fig. 2. The sample was suspended from one end of the balance beam by means of a platinum chain outside the furnace and a long thin quartz fiber on the inside of the furnace. On the other end of the balance beam, the necessary weights were added to counterbalance the sample. In addition, a calibrated chain was added to the balance which was linked directly to the weight recording unit. Control was effected by means of a photoelectric circuit." A parallel beam of light from a strong source was directed onto a small front-surfaced aluminum mirror mounted in the middle of the balance beam and then to a front-surfaced mirror mounted on the ceiling of the room. The beam was then reflected onto a front-surfaced right prism at a distance of 9 ft from the balance

Jan 1, 1957

By Clarence Karr

In 1955 the Federal Bureau of Mines established a low-temperature tar laboratory at its new Appalachian Experiment Station in Morgantown, W. Va. The objective of the laboratory is to investigate the yields and chemical and physical properties of tars from low-temperature carbonization of coal, to investigate means of economically upgrading these tars, and to make available to industry and the public essential data for increasing coal utilization through the establishment of a new coal-chemical industry, based on the utilization of low-temperature tars. Because of the obvious economic significance of phenols, as well as the relative ease with which they can be separated and analyzed, initial research has centered mainly around this class of tar constituents. It was realized early that no listing of phenols and their physical properties existed that included enough compounds to be practicable. The purpose of this paper is to make such a compilation available.

Jan 1, 1957

By Herty, C. H.

One of the numerous requirements of many grades of present- day steel is that the steel shall be free from non-metallic inclusions. These inclusions may be composed of oxides, sulphides, complex oxy- sulphides, and nitrides, which enter the steel with the furnace charge, result from sulphur absorption from the furnace gases, or are formed in the steel during the deoxidation process. Although few' data are available which indicate in any quantitative manner the specific effects of inclusions in steel, there is a large mass of circumstantial evidence which points to the advisability of producing steel free from these impurities for many purposes. At the present time there is a growing feeling among metallurgists that non-metallic inclusions should be divided into two distinct types: (I) those readily visible under the microscope at ordinary magnifications; and (2) those in colloidal suspension or in solid solution. Both types are profoundly influenced by the character of the charge, the manipulation of the furnace slag, and the method of deoxidation. The work described in this bulletin deals primarily with inclusions visible under the microscope at ordinary magnifications, but the steels made by the various methods of deoxidation are being used LO study certain effects which may be ascribed to the second classification, named above. This latter work will be the subject of further bulletins on the effect of deoxidation practice on the physical properties of the steels involved.

Jan 1, 1957

By D. D. Pollock, D. I. Finch

Relationships between the compositions of specially prepared manganin-type alloys and some of their electrical properties have been established. Empirical equations, based upon the electronic configurations of the alloying elements, are given which describe the resistivity, temperature coefficient, peak temperature, and thermoelectric power of Cu-Mn-Ni-Fe alloys at approximately room temperature. Calculations based upon these relationships are correlated with experimental data. SECURING suitable alloys for the construction of stable resistors, for use in precise electrical measuring devices, has been important ever since the art of electrical measurement was begun. German silver, Pt-Ag, and Platinoid are examples of some of the alloys in early use. These early alloys were un- satisfactory for one or more of the following reasons: l—insufficient stability of electrical properties with time, 2—poor reproducibility of electrical characteristics from melt to melt, 3—excessive temperature coefficients of resistance, and 4—excessive cost. Weston introduced the Cu-Mn-Fe and Cu-Mn-Ni-Fe alloys of the type now generally known as manganins. His patents are believed to represent the first disclosure of any alloy with a negative temperature coefficient of resistance. After this work, the German company, Isabellenhutte, in conjunction with Feussner and St. Lindeck, produced alloys of

Jan 1, 1957

By F. E. Jaumot, R. L. Smith

Self-diffusion in zinc has been used as an instrument for comparison of the absorption and sectioning techniques as a means of studying diffusion. Single crystal as well as poly-crystal samples were used asanda the temperature range of diffusion extended from 200° to 415°C. For temperatures above 200°C, the data indicate that the results obtained from the absorption technique agree with those obtained from the sectioning technique. The effect on the values of the diffusion coefficient of electroplating vs evaporation as a means of applying the tracer was investigated and no significant difference observed. It was found that an excess or deficiency of tracer did not materially affect the results obtained from the sectioning technique, but invariably caused errors with the absorption technique. NEARLY all self-diffusion experiments and many alloy diffusion experiments have employed radioisotopes as the instrument for following the diffusion. Of the various techniques in which radioisotopes are applicable, the two most widely used are the sectioning and absorption techniques. In the former, the diffusion coefficient is obtained from a curve of log concentration vs the square of the mean penetration depth. In the latter, the diffusion coefficient is calculated from a knowledge of the decrease in activity at the surface after diffusion. In spite of the importance of knowing the reliability of the diffusion data and the widespread use of these two techniques, they had not been directly compared experimentally on the same samples. Thus, such a comparison was worthwhile. The specific system chosen for this comparison was the self-diffusion of zinc, since the metal was readily obtainable in high purity, single crystals were easily grown, and the anisotropic features of the diffusion added an additional factor of interest to the comparison. Self-diffusion in both single and polycrystals was investigated, since the possibility existed that grain boundaries and grain boundary diffusion might produce different effects for the different techniques. Also, the effects of electroplating vs evaporation as a means of applying the radioactive tracer, and the effects of applying an excess or deficiency of tracer material were studied. The general experimental procedures and the mathematical analyses of both techniques have been described previously in some detail, and only those points essential to an understanding of the present work will be discussed here. The mathematical analysis of the sectioning data requires only a knowledge of the solution of Fick's equation. where C,, is the initial concentration, C is the concentration at depth x, D is the diffusion coefficient, and p is the absorption coefficient of the solvent metal for the radiation from the solute. Having obtained F from the experiment, the value of z can be read from a plot of F vs In z, and D can then be calculated if is known. The necessity of knowing the absorption coefficient causes most of the criticism of the absorption technique. It is very difficult to measure accurately under the conditions existing in the diffusion experiment, but it is absolutely necessary, as will be indicated briefly later. Portions of this problem have been discussed in detail elsewhere." The difficulties involved in the measurement of the absorption coefficient arise from three principle factors: the physical characteristics of the absorber, the geometry, and complex radiation spectra. The first two are heavily dependent upon the third. If

Jan 1, 1957

The early history of the mine is traced from the beginning of shaft sinking in 1886 to the purchase by the Broken Hill Proprietary Co. Ltd. in 1949. A necessary preliminary to mechanisation of the Borehole Seam was development of the Young Wallsend seam, andthis development is described. Surface reorganisation and coal handling arrangements are dealt with in detail. Then follows a description of the Borehole Seam mechanisation, the provision of power supply for this purpose, arid pumping arrangements in themine.INTRODUCTIONStockton Borehole Colliery is in the Parish of Teralba, between the townships of Teralba and Boolaroo, and about 12 miles from Newcastle. The colliery holding, a freehofd area of 2,560 acres, was apparently an original land grant when acquired by Teralba Co-operative Coal Company who decided to mine for coal and named the mine "Teralba Colliery." Shaft sinking was commenced in 1886 but was delayed by financial and water troubles to such an extent that it was not until 1901 that the Borehole Seam was reached.Coal was won until 1904 using a single 16 ft. diameter shaft, ventilation being achieved by means of a wooden boxing down one side of the shaft. This collapsed, and operations ceased until the mine was taken over in 1906 by a company known as "Borehole Colliery Limited," the principal stockholder being the Stockton Coal Company. It renamed the mine "Borehole Colliery." This new company immediately commenced sinking a 13 ft. diameter air shaft. In 1908 the Stocktol1 Colliery at Stockton was abandoned, and during the following year much of its equipment was transferred to Borehole Colliery. The name was again changed becoming "Stockton Borehole Colliery." From this period on, coal was produced from the Borehole Seam by...

Jan 1, 1957

By W. Rostoker, D. W. Levinson, A. Yamamoto

The influence of carbon on tensile strength, tensile ductility, transformation kinetics, and grain growth characteristics of selected Ti-Mo base alloys was studied. No systematic influence of carbon in tensile strength or significant deleterious effect on tensile ductility was observed. There was a marked increase in transformation rate due to carbon. Dispersed carbides exert a marked inhibiting effect on grain boundary migration, and thus effectively prevent grain coarsening during solution treatment in the ß phase field. AS part of a research program directed toward the illumination of factors governing modes of transformation, transformation kinetics, and mechanical properties obtainable through these transformations by heat treatment, Ti-Mo base alloys were selected for study. The binary system is a characteristic phase diagram type which has been studied in some detail', ' in relation to transformation kinetics and mechanical properties. Although carbon bearing alloys have acquired a bad reputation, the possibilities of melting titanium under conditions which occasion some carbon pickup are very attractive. It is therefore of considerable importance to know whether carbon, present as a dispersed carbide phase, is actually deleterious when all other detrimental factors are minimized. Basic alloy compositions containing nominally 3, 5, 7, and 11 pet Mo were prepared with systematic carbon addition up to 1 pet by weight. Various of these alloys were subjected to a series of critical and definitive experiments to delineate the effect of carbon on the transformation behavior and associated mechanical properties. Experimental Procedure Alloys were prepared from 115 Bhn magnesium-reduced sponge titanium. This sponge analyzed ap- proximately 0.05 pet C. Ti-Mo and Ti-C master alloys were made by arc-melting the sponge with high purity (99.9 + pet) molybdenum and spectro-scopic grade graphite, respectively. Alloys were then prepared from the master alloys and sponge by double are-melting. One kg ingots were prepared by melting in a nonconsumable electrode furnace. These ingots were forged at 1000°C to '/z in. rods, and cleaned and processed into electrodes for the second melting operation. The final ingots were ground to remove surface defects, then forged again to 1/2 in. or 3/8 in. diam rods for processing to test samples. It is significant that all of the alloys at all carbon levels forged satisfactorily. For convenience, the alloys will be referred to throughout the text by their nominal analyses. Samples for the study of transformation rates were prepared from 1/2 in. diam round stock. They were then solution treated in a helium filled tube furnace at 1000°C for 30 min prior to the isothermal transformation treatments in lead bath furnaces. Temperature control in both cases was within ±3oC. Following the isothermal transformation treatments the samples were water quenched. These experiments were carried out before the general adoption of the resistometric procedure for kinetic studies. The data were therefore obtained entirely by metal-lographic analysis. M, temperature was also determined by the metallographic method. Shoulder-type tensile test pieces were machined from heat treated, 1/2 in. diam slugs to provide a 0.252 in. test diam and a 1 in. gage length. The isothermal-type heat treatments were chosen from previous data' to provide three levels of strength and ductility.

Jan 1, 1957

By Nicholas J. Grant, H. C. Chang

TRANSCRYSTALLINE fracture surfaces of the cleavage type have been examined by microscopy and X-rays for several metals.' These investigations revealed that the fractured surfaces were not flat and invariably had cleavage and other deformation markings on them. On the other hand, the study of inter crystalline fracture surfaces has been limited. Perryman, in a recently published paper on the inter crystalline fracture of ß-brasses,' found that a thin layer of heavily deformed metal was invariably associated with these surfaces. Furthermore, the thickness of this layer was found to depend on the orientation of the grain boundary surface with respect to the applied stress. The mechanisms of grain boundary sliding and intercrystalline fracture have been presented in two previous papers,which described certain aspects of the deformation of a 20 pct Zn-A1 alloy. It is the purpose of this paper to present some observations on the structure of intercrystalline fracture surfaces and to correlate the structure of such surfaces with the mechanism of intercrystalline fracture. Experimental Techniques—The high purity 20 pct Zn-Al alloy was generously supplied by the Research Laboratories of the Aluminum Co. of America. Two sizes of specimen were used; the first had two parallel flat surfaces of dimensions 1x0.17x0.09 in. and the second was round with a 0.25 in. diam. A grain diameter of 1 to 3 mm was obtained by annealing the specimens at 1000°F for 24 hr. The specimens were then air cooled. The specimens were subjected to creep at 500°F and 2300 psi. The rupture times ranged from % to 3 hr, with one room temperature tensile test. It has been mentioned previous1y" that the intercrystalline fracture surfaces of this alloy, when tested under the conditions given above, are sharply defined. In the optical examination of the fracture surfaces, whenever possible, magnifications of at least X250 were used. The locations of the regions examined, both optically and by X-rays, were selected to give several fracture surface orientations with respect to the stress axis and to the specimen surfaces. This was possible for the X-ray studies since the grain diameters were large compared to the X-ray beam. A film to specimen distance of 3 cm, a 1 mm pinhole and Cr radiation were used for the Laue back reflection pictures.

Jan 1, 1957

By V. J. Decarlo, J. J. Gilman

POLISHING pure zinc differs somewhat from polishing less reactive metals. The problem is not that of finding a suitable reagent, but rather of producing the polish in such a way that the surface remains polished after it is removed from the polishing bath. In other words., the anodic film that is vital to the polishing mechanism' must be tightly adherent and nonporous. It is usually desirable that it be thin. Polishing solutions consist of proper proportions of an acid and a strong oxidizing agent. In electro-polishing, the external circuit acts as the oxidizing agent. The proportions are critical because the essential surface film must be maintained at approximately constant thickness during the polishing process. In the case of zinc, chiefly two oxidizing agents, chromic and nitric acids, have been used. The simplest polishing reagent is concentrated nitric acid. However, it has certain disadvantages. It tends to pit: an excessive amount of heat is evolved during polishing; and the oxide film that it produces is not very stable, so that the polished sur-

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published 1942-45 as a series of seven miners' circulars (Nos. 51-57). The course has been broadened, revised, and brought up to date and is being published as a similar series of seven miners' circulars on accident prevention at metal and nonmetallic mines. These circulars are: 1. Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1957

By W. L. Crentz

San Juan County, which occupies the extreme northwest corner of New Mexico, contains large reserves of coal in the Fruitland formation and in the Menefee formation of the Mesaverde group. The coals have bright luster, are brittle, and break easily in handling. All mines sampled are in the La Plata-Fruitland and Rio Chaco districts of the Durango-Gallup coal field. This large area, all within San Juan County, contains numerous coal beds 5 to 15 feet thick. Ellis2/ mentions the Carbonero (Fruitland in this report) bed in the La Plata-Fruitland district attaining a thickness of 36 feet. This bed has been correlated with the Carbonero bed, formerly mined at Carbon Junction, near Durango, Colo. During the field investigation covered by this report, no operating mine in the Fruitland bed was working a bed thickness of more than 15 feet.

Jan 1, 1957

By J. P. Powell

The importance of recovering more oil from known petroleum reserves has placed increasing emphasis on the application of secondary producing methods. One of the most successful of these has been the injection of water into depleted oil reservoirs. Water flooding is now recognized as a valuable conservation measure that not only prevents the premature abandonment of stripper leases but also is credited with reviving operations in many oil-producing areas previously abandoned. The injection of water into an oil-producing zone as a method of stimulating oil production was legalized in Kansas in 1935. Although water flooding had been attempted previously in other parts of the State, 1935 marked its introduction into the shallow stripper area of eastern Kansas. Two years later flooding was begun in the five-county area that is described in this report. Figure 1 is a map showing the water-flood areas in Allen, Bourbon, Crawford, Labette, and Neosho Counties, Kans. To July 1, 1955, the 77 projects in the oil fields of these 5 counties are credited with recovering an estimated 12.3 million barrels of oil that would not have been produced by methods used previously. These projects are expected ultimately to cover 10,700 acres, of which only 5,400 has been flooded to date.

Jan 1, 1957

By H. W. Paxton, C. C. Busby

IT has been shown previously' that strain aging can markedly improve the tensile properties of low carbon martensites, especially the yield-tensile ratio, without seriously affecting the ductility. In view of interest in high strength steels, an investigation has been made of the effect of strain aging following tension or rolling on the tensile properties of A1S1 4340 in an attempt to obtain a tensile

Jan 1, 1957

The Aberfoyle Tin Mine lies on a wide sloping bench about 2,000-2,500 ft. above sea level, at Rossarden, 14 miles north of Avoca, in north-eastern Tasmania. The quartz-cassiterite veins were discovered in 1916, but mining did not begin until 1926. Trenching revealed seven small tin-bearing veins within a width of 57 ft. of Palaeozoic slates and sandstones, and it was assumed that the mineralization extended beneath the adjacent cover of Permian strata, but the presence of the main vein system (the 26 Vein System) was not suspected until the Aberfoyle Fault was discovered late in 1928.The mine has now been developed on thirteen levels, to a depth of 1,350 ft. The lower limit of economic mineralization appears to lie at about the ll-level, which is 1,060 ft. vertically below the concealed outcrop of the main veins. Production of tin and tungsten concentrates began in 1932, and to date more than 550,000 tons of ore have been mined for a recovery of 8,856 tons of tin concentrates, and 3,056 tons of wolfram concentrates, valued at approximately £6,500,000.This paper reports part of an investigation undertaken by the Mineragraphic Investigations Section of C.S.I.R.O. to study the mineral composition of the ore in relation to the apparent failure of cassiterite and wolfram mineralization to extend below the present working limits of the mine, and was first issued as Mineragrapnic Report No. 639.GENERAL GEOLOGY:The deposit consists of a series of quartz veins in a northsouth trending sheeted zone, transecting folded slates and...

Jan 1, 1957

By K. E. Stanfield

The Bureau of Mines oil-shale program, initiated in April 1944, is concerned with the future utilization of oil shale in the United States as a source of liquid fuel. One phase of this program is the accumulation of information on the location, extent, and richness of oil-shale deposits that may be suitable for processing to oil and related products. A previous publication5/ presented, by means of logs, the oil yields of sections of the largest known oil-shale deposit in this country -the shales of the Green River formation occurring in adjoining portions of the states of Colorado, Utah, and Wyoming. This present supplementary report presents the oil yields of cores from 48 holes drilled during 1952 to 1954 in the Green River formation of Colorado, which is distributed over an area of more than 1,000 square miles. The oil yields of the 48 oil-shale sections, involving the assay of 9,651 samples, representing 22,451 feet of core, are presented by means of logs. In addition, the oil yields of samples comprising the maximum sections of 15 gallon-per-ton shale are tabulated for these cores and for the 28 cores from Colorado which were logged in the previous report.

Jan 1, 1957

By James Westfield

A brief resume follows of some recent activities of the Division of Coal-Mine Inspection that have had a favorable effect on health, safety, and the reduction of injuries at coal mines: 1. The Federal Mine Safety Code for Bituminous-Coal and Lignite Mines of the United States was issued originally by the Director of the Bureau of Mines on July 24, 1946, after consultation with management and labor representatives of the coal-mining industry. The code has been used by Federal coal-mine inspectors during their inspections of bituminous-coal and lignite mines as a basis for determining the existence of unhealthful and unsafe conditions and practices in these mines. A revised code was issued by the Secretary of the Interior October 8, 1953, following further consultations with representatives of management and mine workers, and was incorporated by reference in the 1952 and subsequent bituminous-coal wage agreements. The agreement of May 29, 1946, between the Secretary of the Interior, acting as Coal Mines Administrator under authority of Executive Order 9728, and the United Mine Workers of America, covering bituminous-coal and lignite mines in Government possession, charged Federal coal-mine inspectors with the responsibility of making periodic investigations of the mines and reporting to the Coal Mines Administrator any violations of the Federal Mine Safety Code. The inspectors were active in making prompt investigations of hazardous mines that had been closed by order of the Coal Mines Administrator to determine if enough improvements had been made to allow the mines to reopen. Federal coal-mine inspectors also had temporary authority to close mines they found to be imminently dangerous, but such authority (under Executive Order 9728) was removed on June 30, 1947, when Government control of the mines was terminated.

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942-45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date, and it is being published as a similar series of seven miners' circulars on accident prevention in metal and nonmetallic mines. These circulars are: 1. Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942-45 as a series of seven miners' Circular (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date and is being published as a similar series of seven miners' circular pros. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1957

By E. P. Carman

This report is the 20th in a series summarizing Bureau of Mines research and technologic work on coal and related investigations; it is the second4/ to be issued on a calendar-year basis. Previous reports related largely to publications by Bureau authors during the reporting period. This one discusses the publications issued during 1955 and in addition describes briefly the work in progress during the year. Further details on the published work may be found by referring to the publications cited in the footnotes. The Bureau continues to direct its research and technologic work on coal toward safer and more efficient mining, improved preparation, and more effective utilization, with the ultimate twin goals of promoting conservation and insuring that coal will make its maximum contribution to the Nation's industrial capacity. Significant advances toward these goals were made in 1955.

Jan 1, 1957

By T. A. Klinefelter

ONE OF THE many services rendered by the Federal Bureau of Mines is the identification and general examination of ore and mineral samples. Many of these, coming from almost every State in the Union, are clay and shale samples. Other Government agencies, State geologists, universities, and other laboratories are often requested to make similar examinations. This publication describes methods of testing these samples. An earlier paper, published in 1943, described Bureau of Mines methods of testing such clays.3 This paper was to be followed later with another (part II) that would describe much more thorough testing than did the rather general outline of part I. Part I has been out of print for some time and needs revision, and part II was never written; hence, the present publication is designed to include part I and also those additions intended as part II. The tests presented in part I were simple, requiring only the ordinary equipment to be found in any good chemical laboratory. The second publication was to include a greater number of test procedures and information on increasing the accuracy and precision of those previously given.

Jan 1, 1957