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By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By Walter C. Lorenz

In connection with its renewed study seeking solutions to problems created by release of acid water from bituminous coal mines, the Bureau of Mines recently surveyed reports already written on the subject. This publication is based on that search. The Problem Poor distribution of water is evident on an ordinary geographic map of the United States. The more abundant supplies of surface water appear to be centered in the northeast, the southeast, and the central humid areas of the country. It is in the midst of this abundant surface water, in the Ohio River Valley, that most of the bituminous coal is mined. Varied industry has located in the valley to use the coal and the river. The coal is a source of power and o raw material. The river provides transportation for raw and finished materials; equally important, it provides the water that is used for cooling and processing in manufacturing. It also serves as a vehicle for the disposal of waste.

Jan 1, 1962

By Alla D. Mah

The need for more and better basic thermodynamic data for the oxides of many of the rare metals is evident to anyone who attempts thermodynamic calculations involving these substances. In continuation of a Bureau of Mines program to meet this need, this paper reports new experimental values of the heats of formation at 298.15° K. of the hexagonal crystalline variety of germanium dioxide and germanium dioxide glass. The values were obtained by means of combustion calorimetry and sodium hydroxide-solution calorimetry. The calorimetric results also made possible the derivation of values for the heat and entropy of fusion of hexagonal germanium dioxide at its melting point. The newly measured data were combined with previously known entropy and high-temperature heat content values to obtain heats and free energies of formation of germanium dioxide (in the hexagonal crystalline, glassy, and liquid states) over the temperature range from 298.15° to 2,000° K.

Jan 1, 1962

By S. A. Montague

In spite of the many new insulating materials, both synthetic and manufactured, that have been put on the market since the end of World War II, and notwithstanding the many millions of dollars applied to the development of synthetic mica, natural block mica1 is still a most indispensable insulator in various electronic components. It will remain so, barring some spectacular break-through in research that might provide a substitute fully acceptable as a replacement for mica in all of its superior properties. But this is not to say the future for mica is assured, or free from serious problems. Technological advances have created problems requiring a solution to be found if future requirements are to be filled.

Jan 1, 1962

By Dexter C. Hatch

At MacIntyre Development of the National Lead Company, Taha s, New York,, the flotation plant was set up to recover ilmenite from the finer size fraction of the ore that cannot be efficiently treated in the main gravity-magnetic separa¬tion process. It was later expanded to handle the reground middlings from the tables wetherill magnetic separators. The ilmenite-magnetite ore is ground to minus 20 mesh in five 6 x 12 ft. rod mills in closed circuit with DSM screens. The minus 20 mesh screen undersize is pumped to four parallel sections each consisting of two rougher wet-magnetic separators and one cleaner separator for magnatite removal. The screen undersize from the fifth section is distributed to all four sections. The magnetite removed in the roughers is pumped back to the cleaners and the cleaner magnetite is dewatered in rake classifiers and carried by belt to the winter plant or the stockpile area. The nonmagnetic sands from rougher and cleaner magnetic separator are sized for table feed in eight pocket hydraulic sizers. The slime overflows from the Crocketts, the sizers, and the magnetite rakes are collected and pumped to three-inch cyclones for thickening and desliming. The cyclone underflow is the principal flotation plant feed.

Jan 1, 1962

By Sara Jane Boles

In recent years the demand for products of greater refractoriness has placed an ever-increasing emphasis on ceramic materials, including the metallic oxides. Magnesia (MgO) is one of the most important of these oxides, exhibiting, as it does, high electrical resistivity, high slag resistance, and a melting point of 2,800° C. However, magnesia has a tendency to hydrate in the presence of water and to volatilize above 1,500° C. in certain kiln atmospheres and has a comparatively low resistance to thermal shock. Because of these disadvantages, the previously listed advantages inherent in this material have been largely overlooked, and research on magnesia has lagged behind that on oxides such as alumina and zirconia. This bibliography has been prepared in an effort to present to Government and industry a comprehensive picture of the prospects for greater utilization of magnesia as a refractory material in future research. To provide as selective and accurate a collection as possible, the references included cover magnesia in a pure state, not as an additive or in combination with other materials. However, several references discuss the effect of minor impurities (less than 5 percent of the total) on the properties of magnesia, as these papers are considered to be of special importance. A few references to articles on forming techniques are also included, as they are valuable additions to the overall treatment of the subject. The processes used in obtaining and refining the raw materials are adequately covered in earlier publications and are excluded. A number of references are omitted as being of questionable value in enhancing the cumulative study of pure magnesia as an ultra-high-temperature refractory material.

Jan 1, 1962

By Raymond W. Hiteshue

Experiments were conducted al temperatures of 480° to 800° C. and hydrogen pressure of 6,000 p.s.i.g. to determine the effect of coal residence time on the conversion of a high-volatile bituminous C coal to liquid and gaseous products when using a semicontinuous apparatus designed fur rapid heating and cooling of reactants. The objective of the studies at high temperatures was to determine if appreciable quantities of coal could be converted to gaseous hydrocarbons and low-boiling liquid hydrocarbons. Experiments at lower temperatures were designed to indicate shifts in product distribution with respect to temperature and to learn more about the general mechanism of the reaction when using close control of coal residence time. One percent molybdenum, based on m.a.f. (moisture-and ash-free) coal, was used throughout this investigation. At 800° C., 6,000 p.s.i.g., and "zero" residence time) the yield of gaseous hydrocarbons was about 38 percent and the yield of oil about 4.5 percent, based on m.a.f. coal. With IS minutes residence time, under the same conditions, the yield of gaseous hydrocarbons was approximately 80 percent with no increase in yield of oil. Apparently at 800° C., and hydrogen pressure of 6,000 p.s.i.g. coal was rapidly carbonized to char with expulsion of volatiles. Char was then slowly hydrogenated to gaseous hydrocarbons without production of oil.

Jan 1, 1962

By J. Gurland

The effect of four different second-phase additions on the strength of composite alloys with a common matrix was investigated. The four compositions each consisted of 85 pct by volume of silver with additions of 15 pct of either tungsten, molybdenum, tungsten carbide, or nickel. These particular additives were chosen because of their low mutual solid solubilities with silver at room temperature, the alloys consisting essentially of a dispersion strengthened silver matrix in which the second phase is distributed randomly. Test specimens were prepared by a powder metallurgy procedure consisting of ball milling the mixed powders, compacting, and sintering at 920°C for 1 hr in hydrogen. The constituent powders were of CP quality and of particle size between 2 and 10 ?. The compacts were subsequently hot pressed at 1000 psi and 1400° in an Inconel die, coined at room temperature at 60,000 psi and finally annealed and outgassed in vacuum at 800°F. The microstructures of the alloys are shown in Fig. 1, and the microscopically observed porosity grade was A-2 or better as evaluated by ASTM Recommended Practice B 276-54. The properties of the sintered compacts are listed in Table I, and the load-deformation curves in bending are shown in Fig. 2. The samples, of rectangular cross section, were loaded at the center of 58 in. span, and the reported stress was calculated on the basis of linearly elastic behavior in order to allow the comparison of specimens of slightly different dimensions. It is apparent that the tungsten, molybdenum, and tungsten carbide alloys exhibit very similar deformation curves. The moduli of elasticity were determined from the slopes of the stress-deflection curves at small loads. The measured values agree quite well with those calculated by the strength of materials approximation proposed by Paul1 for the elastic constants of mixtures, the calculated values being 15.0, 15.0, 17.4, and 13.4 million psi, respectively, for the tungsten, molybdenum, tungsten carbide, and nickel combinations with silver. The strength of the Ag-Ni composition is appreciably lower than that of the other three alloys. The discrepancy between the two groups is accounted for by the following characteristics of deformation and failure which were observed microscopically during the tests: A) The deformation of the W, Mo, and WC alloys did not involve the second phase particles to any appreciable extent. Slip and fracture took place in the silver-rich matrix alone, although the fracture path generally skirted the particles by favoring the phase boundaries. The deformation proceeded according to the following sequence: 1) formation of small, discontinuous microcracks in areas of the matrix adjacent to a particle, 2) general slip in the matrix and extension of cracks, 3) failure of specimens by propagation of cracks through matrix. The near coincidence of the 3 load-deflection curves suggests that the nature of the second phase particles does not decisively influence the plastic behavior of composite alloys of this composition as long as the particles do not undergo any considerable deformation themselves. B) A markedly different behavior was exhibited by the Ag-Ni composition where the relatively low flow strength is associated with the low yield strength of the nickel grains. Slip in the nickel grains was first observed at a stress of approximately 10,000 psi, although failure, at a later stage, took place by the propagation of cracks through the matrix. The ductility of this aggregate, in which both components deform plastically, is appreciably greater than that of the elastic-plastic composites. In summary: 1) The measured values of the moduli of elasticity of the composite alloys under discussion are in good agreement with the "strength of materials" approximation proposed by Paul.' 2) The overall plastic behavior of these particle-strengthened alloys is unaffected by the nature of the second phase particles, if the latter remain elastic. This work was supported by the Office of Naval Research. The experimental results are presented

Jan 1, 1962

By E. D. Calvert

The objective of this research was to examine variations in melting and forging practice for four titanium-base alloys and to determine their effect on the resultant product. Of particular interest was the evaluation of the skull-casting technique. The data should serve as a guide to producers and consumers of titanium products. Physical properties of four titanium-base alloys in ingot form and in sheet form were evaluated and correlated, where possible, with variations in the melting and casting procedure. Consumable-electrode melting was used throughout, but arc current and furnace backfill pressure were varied, and ingots were formed both by melting directly into a water-cooled copper mold and by skull melting followed by pouring into a graphite mold. Alloying metal additions for the alloys tested were (1) 8 percent manganese, (2) 6 percent aluminum and 4 percent vanadium, (3) 6 percent molybdenum and 2 percent aluminum, and (4) 16 percent vanadium and 2.8 percent aluminum.

Jan 1, 1962

By Donald E. Redmon

Industrial engineering departments perform staff duties and are most effective when sincerely supported by management. In accordance with the needs and desires of the mining companies involved, various industrial engineering functions have been adopted widely at western metal mines during the period 1950-60. Newly organized departments usually conduct method and equipment studies, work-measurement programs, and establish and maintain production standards. Supervisor-training programs and courses are effective in showing the relationship between supervisory responsibility and the purpose for which industrial engineering is practiced. Industrial engineering staffs of western metal mines are composed predominantly of personnel from within the companies. Experienced industrial engineers, not necessarily experienced in mining, frequently are hired by a company to help establish the department. Management consultants frequently are called upon to advise management and instruct department personnel in industrial engineering practices. Some departments have developed satisfactory industrial engineering programs without benefit of formal industrial engineering training or advice.

Jan 1, 1962

By Howard P. Hamlin

This Bureau of Mines report is concerned with the testing procedures for evaluating clays, shales, and slates for lightweight aggregates using the rotary-kiln method of production. To meet the increasing demand for light-weight concrete, rapid, accurate methods for appraising raw materials for light-weight aggregate are needed. Preliminary tests were made on samples of clay, shale, and slate, using laboratory equipment, and the data were used to establish operating conditions for pilot-plant-size rotary-kiln tests. Lightweight concrete was made from the processed aggregates and the properties determined. The results show that the laboratory data can be used to guide rotary-kiln testing, and, with the exception of sampling, a complete appraisal of a raw material for lightweight aggregate concrete can be made in 3 days by the methods described in this report.

Jan 1, 1962

By J. R. Nettle

The development of a process for upgrading offgrade titanium metal by electrorefining in molten salt led to an investigation of the electrotransfer characteristics of selected metals when alloyed with the titanium to be refined. Previous tests on seven binary titanium alloys showed that the degree of transfer of the alloying constituent depends on the constituent and on the operating procedurese.5 This report describes tests on electrorefining ternary mixtures of titanium with selected metallic elements. Ten alloys were prepared from high purity titanium and 2-1/2 percent of each of the metal pairs selected from the same elements used in the binary study; manganese, vanadium, chromium, zirconium, tin, molybdenum, aluminum. Operating variables were similar to those investigated in the binary alloy study that gave minimum alloy metal transfer. The data presented indicate the transfer characteristics of the various metals and combinations tested relative to each other.

Jan 1, 1962

By Arthur R. Rattew

In conjunction with the research study of the Coronation Mine recommended by the National Advisory Committee on Research in the Geo-logical Sciences and coordinated by the Geological Survey of Canada, Canadian Aero Service Limited per-formed a detailed, low-altitude air-borne survey over a block of ground encompassing the .Coronation Mine. The in-phase/out-of-phase air-borne electromagnetic data are com-pared with "horizontal-loop" ground data with reference to: size and nature of conductors detected; criteria in selection of targets for drilling. In-formation provided by Hudson Bay Mining and Smelting Company on their drilling of the numerous conductors in the area is employed in this comparison. The merits of combining a sensitive airborne magnetometer with an air-borne electromagnetic unit are discussed. The magnetic data are considered very important in assessing conductors as prospects for commercial sulphida deposits in this area of numerous electromagnetic anomalies. The "Coronation" survey illustrates

Jan 1, 1962

By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

This report is the 25th in a series summarizing Bureau of Mines research and technologic work on coal and related investigations, and the 7th of these reports to be issued on a calendar-year basis.3 It reviews briefly work in progress during 1960, and furnishes references to publications by Bureau personnel during 1960 and also to a few older papers that were not cited in prior reports of this series. Details about some of the researches mentioned can be found by referring to the publications cited in the footnotes or in the further list in the Miscellaneous section; other phases of work are reported here for the first time and will be covered in more detail by later publications, Coal programs of the Bureau of Mines extend over the wide range of theoretical and applied studies indicated by the table of contents. Fundamental research on coal structure and on the properties of coal will, over a period of time, increase the general knowledge about coal Which scientists and engineers may use in answering practical questions and in solving problems in the mining and utilization of coal. More applied studies are conducted in connection with the developement and evaluation of new mining techniques and the effective processing and utilization of coal and of coal products. Health and safety activities, analyses of coal being mined, and technical advice and assistance to Federal agencies in connection with fuel and boiler-water problems are among the practical services handled by the Bureau.4 5

Jan 1, 1962

By Howard W. Wainwright

This bibliography was compiled by the Bureau of Mines as part of an investigation into the possible utilization of low-temperature coal-tar bases. The bibliography consists of literature and patent references from about 1945 to 1961 and is divided into the following headings: Analysis and Composition; Production, Synthesis, Reactions, and Utilization; and Separation, Purification, and Properties. Although over 1,000 references are included, no attempt was made to insure a comprehensive survey. The literature and patent references are arranged alphabetically by author or patentee. When several publications have the same author they are listed in reverse order of age, with the newest first. An author index is included because secondary authors are not cross-indexed. In almost every instance, the entry is accompanied by a Chemical Abstracts reference for those interested in locating an abstract of the original paper.

Jan 1, 1962

By F. Fraas

ELECTROSTATIC methods are used to separate and concentrate or purify granular particles derived from ores or various synthetic and agricultural products. Compared with other separation methods that require many technological refinements, the electrostatic attraction of fibers, grass, and seeds to charged surfaces clan be accomplished under the most primitive circumstances, and the early development of this method of beneficiation seemed very promising. Precise application of the method to provide high selectivity, however, is a complex procedure, and interest in this method declined. During this period Mr. O. C. Ralston initiated a Bureau of Mines research program oil electrostatic separation. It is the purpose of thins publication to describe the development of the electrostatic method of particle separation from the early beginning to the present resurgence of interest. Most of the information for this description bas been derived from references, a few of which were not available for thorough review. Much information has been drawn from the investitions of the Bureau. Acknowledgments Mr. O. C. Ralston, former Chief metallurgist of the Bureau of Mines, began the research program on the subject and did research on the mils literature. Both Mr. Ralston and Mr. H. B. Johnson, former president of the Huff Electrostatic Separator Co., furnished patent references. A critical review by Mr. F. D. Lamb, Research director, and Mr. M. J. Spendlove, Supervisory metallurgist, Bureau of Mines, College Park Metallurgy Research Center, lifts been of much value in preparing this report.

Jan 1, 1962

By Sara Jane Boles

In recent years the interest in rare-earth compounds as refractory materials has exceeded the available literature on the subject. While some basic properties, such as density and melting point, of the more readily available rare-earth compounds have been reported in the literature, relatively few papers can be found that deal comprehensively and primarily with high-temperature refractory properties and applications of rare-earth oxides, carbides, sulfides, and nitrides. Therefore, this bibliography has been pre-pared for the use of the ceramic industry as a guide for locating and utilizing the scattered and frequently fragmentary information available. The term "rare earths", as applied in the literature search for this bibliography, is understood to include the following elements: cerium, dysprosium, erbium, europium, gadolinium, holmium, lanthanum, lutetium, neodymium, praseodymium, samarium, terbium, thorium, thulium, uranium, and ytterbium. (On the periodic chart, these elements appear as numbers 57 through 60, 62 through 71, 90, and 92.) It is emphasized that many of the abstracts included are from papers in which the rare-earth compound or compounds are treated along with several other ceramic materials, are mentioned only secondarily, with primary interest placed on a more commonly used refractory material, or are used as part of a mixture of materials formed experimentally and reported on in the paper. As the better known rare-earth materials, such as the oxides of uranium, thorium, and cerium, appear more frequently in the literature, they also appear more frequently in this collection. Articles abstracted include only information on the basic properties that are of interest to the refractories investigator. References to crystal lattices and related topics are generally excluded from this publication. The temperature 1,500° C. has been set arbitrarily as the lower limit for reported data on thermal properties. However, because of the scarcity of information, some reports are included in which data are limited to those obtained at lower temperatures. Many of the articles abstracted include lists of references that will be of additional assistance in pursuing specific lines of investigation.

Jan 1, 1962

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By Joseph H. Bilbrey

COBALT is a silvery gray metal which closely resembles nickel in appearance and properties although it is somewhat harder and more brittle. It is rather widely disseminated and is estimated to make up about 0.001 percent of the earth's crust as compared to 0.020 percent for nickel. Cobalt, one of the four ferromagnetic elements, is used for many magnetic applications. It is oxidation resistant, a property which when coupled with its moderately high melting point of 1,495° C., makes it useful in high-temperature applications. Although cobalt had been used by man as a coloring agent for glass and other ceramic products for 4,000 years, it was not isolated as a metal until 1742 and not established as an element until some 40 years later. Early in the 20th century, cobalt began to be used in alloys, and soon these applications displaced ceramics as the major consumer of cobalt. The use of cobalt in alloys gave considerable stimulus to production, and the world output of cobalt increased rapidly, rising from 400 tons in 1920 to 1,400 tons in 1930 and 5,500 tons in 1940. With the advent of the jet plane in the mid 1940's and the consequent increased need for cobalt-bearing high-temperature alloys, cobalt production again increased, reaching 7,900 tons in 1950. The increased demand for cobalt during the Korean war coupled with a large demand for stockpiling caused world production to more than double within the next 10 years, reaching a peak of 17,300 tons in 1959.

Jan 1, 1962