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By Bernard Lewis

This report summarizes fundamental research end technical studies conducted in the Explosives and Physical Sciences Division, Region VIII, of the Bureau of Mines in the 2 years July l, 1950, to June 30, 1952. It is the fifteenth of a series of, ordinarily, annual reports whose aim has been to provide the reader with a resume of the research results that have appeared in published form during each fiscal year under the authorship of members of the staff. These are referred to throughout the report. ACKNOWLEDGMENTS Acknowledgments art, made to the following members of the Division wider whose mediate supervision the described studies were carried out. Stuart R. Brinkley, Jr., chief, Mathematical and Theoretical Physics Section, and special assistant to the chief of the division.

Jan 1, 1953

By J. B. Gayle

In a modern blast furnace, production depends, to a large extent, on the rate at which the furnace gases can be forced through the charge. Since these gases must make their way through the voids between particles of coke, ore, and limestone, the size and size distribution of the stock-column materials are of considerable importance. Also, because the coke pieces support the weight of the overburden and provide the majority of the voids through which the gases pass, their ability to withstand the shattering and abrading forces to which they are subjected should be related to the maximum obtainable production for any particular furnace. Although the wide acceptance of this point of view is indicated by the ever-increasing demand for stronger and more uniform blast-furnace cokes, economic considerations demand that a quantitative evaluation of the relation between coke quality and blast-furnace performance be made available to the industry at the earliest possible date. The following studies of size-distribution patterns and breakage processes were, therefore, conducted as a part of a preliminary investigation intended as a basis for future studies of the relation between coke quality and blast-furnace performance. The major findings may be summarized as follows: 1. New evidence for the presence of two independent distributions of sizes in run-of-oven cokes has been obtained, and a method for characterizing and estimating the relative importance of the individual distributions has been demonstrated. This method has also been used to study the different types of degradation taking place during the tumbler test.

Jan 1, 1954

By Alfred Traverse

The Brandon lignite is a small deposit of very low rank coal near the village of Forestdale in the town of Brandon, Vt. It occurs in association with other sediments, principally sands and silts. This lignitic coal has attracted considerable scientific interest since the middle of the 19th century because of the abundance of fossils in the sediment and the rarity of lignite in New England. A cooperative investigation has been developed by E. S. Barghoorn, W. Spackman, and the author in which different phases of the problem have been worked on in a coordinated research program. This paper presents results of an investigation of the very abundant fossil pollen and spores and some other microfossils of the deposit. The studies on which this manuscript is based were made in large part at Harvard University in partial fulfillment of the requirements for a Ph. D. degree.

Jan 1, 1955

The complex organic chemicals in coal differ from those in petroleum mainly by the ratio of carbon atoms to hydrogen atoms; this ratio is about 2 for coal and 1 for petroleum. By changing the ratio, coal can be converted into compounds similar to those found in petroleum. In. very simplified form, omitting here the special conditions required, the paths by which this can be done are: [ ] Part or all of the coal is first gasified by reaction with steam and oxygen, either in a gasifier or while the coal is still in place underground. The resulting gas is mainly hydrogen and carbon monoxide, with impurities that .must be removed before further processing by one of the following routes.

Jan 1, 1959

By J. B. Zadra

Tungsten metal, chemically equivalent to commercial grade, is produced by electrolysis of impure tungsten compounds or scheelite in an alkali, phosphate or borate electrolyte. A preliminary investigation of fused-bath electrolysis shows the effect of electrolyte composition, temperature, and current density on current efficiency, yield, crystal structure, and purity of product. Experiments show that tungsten can be electrowon from scheelite in a fused alkali, phosphate, or borate bath with similar results. Studies on electrolyte composition show that the addition of sodium chloride is essential to both electrolytes in treating scheelite. Although its main function is to react with or flux the CaO, it also increases the bath fluidity. Temperature studies revealed optimum ranges between 900° and 1,100° C.; 900° C. proved satisfactory for tungsten trioxide, and 950° to 1,050° C. for scheelite. Current efficiencies were satisfactory for all current densities ranging from 10 to 57 a./dm.2. Yields were 400 to 650 g./kw.-hr. over the same current-density range. Crystal size and purity of the product are functions of temperature, current density, and amount of impurities in the electrolyte. Deposited crystals vary in shape from spherical grains to clusters of dendritic hexagonal needles, and in size from smaller than 35 to 570 microns. The purity of the tungsten metal produced ranges from 99.7 to 99.94 percent.

Jan 1, 1959

By J. D. Ramsdell

To obtain information on the effects of cobalt on microstructure and tensile properties of titanium-vanadium-cobalt alloys, the composition ranges of 4 to 16 percent vanadium with 1 to 4 percent cobalt have been studied. The beta phase was not completely retained with vanadium additions up to 16 weight-percent or in the same alloys containing up to 4 percent cobalt.

Jan 1, 1960

By John D. Bardill

A cooperative project between the Bureau of Mines, Department of the Interior, and the Montana School of Mines, investigating results of hydraulic systems for transporting sand slurries for emplacement, was begun in August 1955. In such circumstances, the Bureau provides funds for a fellowship leading to a Master of Science degree as well as available instruments, tools, supplies and equipment. The School provides the ore-beneficiating laboratory with its equipment for use as a pilot plant. The success of a hydraulic backfilling method employing mill tailings depends largely upon the physical characteristics of the tailings. One of these characteristics is size distribution, especially in the finer size ranges. When being emplaced underground, almost impervious layers of slimes separate from some types of mill tailings containing a high percentage of slimes and settle on the top of the sand fill. These coatings may be so dense that the water in the slurry cannot percolate through them for proper drainage. Successive layers of fill in a stope, each with an impervious coating on top, sometimes build up a hydrostatic head, creating pressure on the bulkheads. This may cause breaks in the lining material, inducing sand runs and flooding the level and sumps below. Deleterious slimes flocculated and disseminated throughout the sands should help prevent the formation of impervious slime layers, increasing percolation and settling rates.

Jan 1, 1960

By M. Vanpée, H. G. Wolfhard

Jets of hot gases issuing into explosive gaseous mixtures are efficient agents of ignition . The ignition temperature is defined as the temperature of the jet as it enters the cold explosive mixture which is just high enough to produce ignition . Such data have been published recently.5/ The investigators note especially that no correlation seems to exist between hot - gas ignition temperatures and spontaneous ignition temperatures , although there is a rather loose relation with limit flame temperatures . Before a more quantitative theory of the hot - gas ignition process can be attempted effectively , several questions must be answered : ( 1 ) Can the reactions leading to ignition be described by an Arrhenius type activation energy? ( 2 ) Is ignition preceded by an induction period ? ( 3 ) What is the rate - determining process of the ignition ? (4) And how does turbulence affect this type of ignition ?

Jul 1, 1960

By L. J. Kane

Conventional methods for determining the size of dust suspended in a gas require that agglomerates (clusters of particles) first be broken into particles, but in evaluating industrial dust-removing equipment the size of the agglomerates as they actually exist in the gas stream is far more important. This paper presents results of an investigation by the Federal Bureau of Mines to develop methods for determining the size of dust agglomerates suspended in a gas stream. The studies are part of the Bureau's continuing research on synthetic liquid fuels. The size and size-distribution of agglomerates as they exist when the gas reaches the filter was determined by using a membrane filter in conjunction with a dust count under a microscope. A membrane filter is a cellulosic sheet about 150 microns thick containing millions of holes per square centimeter--holes of uniform diameter that run directly through the sheet without interconnection.

Jan 1, 1960

By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By W. L. Hunter

The research on this report was conducted to obtain information on the feasibility of producing ferro chromium of varying silicon and carbon contents from domestic chromite. Concentrates from the Mouat deposit were chosen because they typify the chromite found in the Stillwater complex, the largest domestic reserve, and are similar in composition to other extensive North American and foreign deposits. Batch-smelting tests designed to produce high-, medium-, and low-carbon ferrochromium were made in single phase and three-phase, electric-arc, steelmaking furnaces. Agglomeration studies were made in a rotary kiln. Continuous smelting tests were made to yield data on the production of high-carbon ferro chromium and low-carbon ferrochromium-silicon. The carbon content of high-carbon ferrochromium was lowered to the medium-carbon range by oxygen injection. Mouat stockpile concentrates were nodulized in a gas-fired rotary kiln using quartz, limestone, and fluorspar additions in the proportion necessary to flux the slag. The nodules were smelted in a continuous test using coal, coal char, and mixtures of the two consecutively as reductants.

Jan 1, 1961

By R. S. McClain

The Federal Bureau of Mines investigated residues from aluminum plants, to determine if carbon could be removed by flotation while recovering fluorine and aluminum compounds for recycling to the reduction process. This publication summarizes studies on samples representing three types of plant waste products, supplied by three aluminum-producing companies. Samples of flue dust, pot skimmings, and pot linings from the various plants all responded to a simple turpentine flotation scheme to reject 90 to 97 percent of the carbon. Aluminum compound recoveries ranged from 42 to 94 percent on the flue dust, were about 95 percent on the pot skimmings, and ranged from 75 to 89 percent on the pot linings. Fluorine recoveries from the same samples ranged from 35 to 63, 92 to 95, and 77 to 86 percent, respectively. The pot linings contained soluble salts of aluminum and fluorine which were recovered by precipitation with sodium aluminate and carbon dioxide gas. Composites of residues from each plant responded to flotation much the same as the individual samples. Aluminum is produced by the electrolysis of alumina in a molten cryolite bath. The electrolytic reduction cell consists of a carbon-lined box containing a pad of molten aluminum which serves as a cathode, a carbon anode, and an electrolyte of molten cryolite in which the alumina is dissolved. Alumina is reduced to aluminum at the cathode, and carbon is oxidized at the anode.

Jan 1, 1961

By F. P. Haver

The Federal Bureau of Mines developed a 10,000-ampere cell to determine the economic feasibility of producing high-purity electrolytic titanium from mill scrap or offgrade sponge. Operating variables were investigated, matetial handling procedures were established, and the cost of electrorefining titanium was determined. The prototype cell produced premium-grade metal (<100 Brinell hardness number (B.h.n.)) from very impure Kroll sponge at a processing cost of less than $0.60 per pound. Refined metal was deposited at the cathode in the form of coarse (85 percent plus 34-mesh), hexagonal crystals of a titanium when the cell was operated an 850° C. A cathode current density of 1,000 amperes per square foot and a molten sodium chloride electrolyte containing approximately 5 percent by weight of soluble titanium were used. In continuous operation, at the optimum number of ampere-hours, (40,000), the current efficiency averaged slightly less than 60 percent. It was possible to supply large enough amounts of electric current for electrolysis to maintain the temperature of the bath, thus reducing overall power consumption to less than 5 kilowatt-hours per pound of metal refined.

Jan 1, 1961

By F. E. Brantley

Research was undertaken by the Bureau of Mines to assess the technical feasibility of smelting cement-copper precipitate in an electric furnace to produce commercial-grade copper. The blister-grade copper produced in smelting was refined by gaseous oxidation and reduction methods to rive a product equal in quality to fire-refined copper. The cement copper used in the study was typical of the material produced in commercial operations. The sample product was received in a partially oxidized state and analyzed 77.5 percent Cu, 3.4 percent Fe, 0.8 percent Pb, 0.05 percent Ni, 0.6 percent Sn, and 0.9 percent S. Smelting tests were made on the precipitate using laboratory-size induction and electric-arc furnaces. Three types of furnace linings were tested during, the investigation: Carbon, including graphite; clay-graphite; and silicon carbide. Although all proved satisfactory, either carbon or graphite was preferred because of their superior refractory properties and low permeability to molten copper. Copper recoveries in the induction and arc smelting tests averaged 92 percent in commercial-grade metal assaying 99.8 percent copper. Refining the molten copper by oxidation and gaseous reduction or by chlorine lancing increased the purity to plus 99.9 percent.

Jan 1, 1961

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 Edwin E. Maust

In response to the ever- increasing demand for high temperature materials, the Bureau of Mines instituted a program for the study and development of superrefractories, One of the major tools obtained for use in this research was an image furnace of the double-paraboloidal mirror type. Although extensive theoretical analyses of solar furnace performance may be found in the literature, comparable detailed information on the double-paraboloidal-mirror image furnace has been nonexistent. This report presents an analysis based on an investigation undertaken to ascertain the limitations and characteristics of the furnace so that it can be used most effectively. The quantitative determination of the energy available at the image, the control of this energy by mans of a 60-inch iris diaphragm, and its variation with position and time relative to the heat source used have all been dealt with in detail. The quantitative results were obtained using a specially designed waterflow calorimeter and these measurements, in conjunction with the theoretical analysis, are used to present a fairly complete description of the furnace and its capabilities.

Jan 1, 1962

By William J. Campbell

The purpose of this investigation was to extend the analytical services which are required for Bureau of Mines programs in developing and evaluating high-purity materials. Determination of trace elements in minerals and ores as an aid in geochemical evaluation and prospecting was considered. Serious consideration should be given to the merits of using the avail- able fluorescent X-ray spectrographic instrumentation and techniques for determining trace elements. Limits of detectability for trace elements in metal, oxide, solution or mineral samples range from 0.1 to 100 p.p.m, depending on the element being determined, overall sample composition, and the complexity of the X-ray spectra; limits of detectability range from 0.01 to 1 microgram for elements that have been preconcentrated by a chemical or physical process, for example, by ion-exchange membrane.

Jan 1, 1962

By Murray Jacobson

Facts obtained by the Bureau of Mines on the dust-explosion hazard in air of materials used in the plastics industry are presented for 313 samples studied in the laboratory. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum energy required for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent ignition and flame propagation, and, in some instances, on the limiting oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle shape, additives, and resin structure on explosibility are discussed. Relative explosibility of the materials is related to the ignition sensitivity and explosion severity and is denoted by an empirical index. Recognition of the degree of hazard will facilitate adoption of adequate measures for preventing ignition and explosion during manufacturing or processing.

Jan 1, 1962

By R. Lincoln

A surplus of vanadium has resulted from the tremendous output of uranium, of which vanadium is a byproduct. More knowledge of the properties and characteristics of vanadium as a pure metal has been needed so that industry can take advantage of its availability and use it according to the best principles of conservation. Besides the problem of utilization, there is the ever present need of finding new materials which will satisfy specific and demanding requirements of science and engineering; vanadium or one of its alloys may possess the latent potential for filling some of these needs. Thus this? research project was undertaken by the Bureau of Mines to determine and examine some of the physical and mechanical properties of pure vanadium. A corallary investigation was the determination of the effect of the interstitial contaminants, oxygen, nitrogen, and carbon, on unalloyed vanadium. The vanadium used for these determinations was principally the product of experimental production of the Bureau. The evaluation of this material, as small quantities became available, provided most of the data that have been obtained.

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