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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 J. L. Konchesky

In gasifying pulverized coal with steam and oxygen, the particle size of the coal fed to a gasifier should be as small as economically possible. A potential way to achieve this advantage is to reduce the particle size of the coal by passing the coal-steam mixture at high velocity through a heated tube coil before the mixture enters the gasifier. To evaluate this method the Federal Bureau of Mines flashed coal-water slurries in externally heated metallic tube coils to determine the extent of size reduction. The first of two different laboratory-scale apparatus reduced the average particle diameter of subbituminous C coal from 190 to 110 microns at an outlet velocity of 330 feet per second (f.p.s.). At the same outlet velocity, a second apparatus reduced the average particle diameter from 250 to 140 microns. An increase in velocity produced more finely divided coal, but variation in temperature and pressure had no effect except as they affected velocity. Virtually the same size reduction was noted for five ranks of coal at equal velocities. The rate of increase in particle-size reduction with increase in velocity decreased with a decrease in particle size. The pulverizing mechanism was concluded to be abrasion of the particles with each other and with the tube wall.

Jan 1, 1961

By T. A. Sullivan

The work described in this report was undertaken to evaluate and develop techniques for determining the oxygen content of titanium and titanium alloys. Early investigations of volatilization techniques involving halogenation were unsuccessful. Later efforts were concentrated on evaluating vacuum fusion and inert-gas fusion techniques. Two vacuum fusion methods and an inert-gas fusion method were found to be satisfactory in the 0.02 to 1.00 pct., oxygen range. These methods are described in detail. The coefficient of variation by any of the three methods is approximately 5 pct, While the main portion of this paper is devoted to the vacuum and inert-gas fusion methods, a resume of other suggested methods for analyzing titanium for oxygen also is given. INTRODUCTION The Federal Bureau of Nines has conducted research on titanium metal since 1938. This research included development of the Kroll process for the production of titanium (2)4, various sodium reduction processes for making titanium metal and lower valent titanium chloride-sodium chloride mixtures (17), and a fused salt electrolytic process for Me production of high-purity titanium metal and the recovery of titanium by electrorefining from off-grade materials (20).

Jan 1, 1961

By Joseph A. Sutton

This study was undertaken by the Bureau of Mines to determine whether the sulfur-oxidizing bacterium Thiobacillus thiooxidans could use sulfur compounds to produce sulfuric acid in sufficient quantities to leach valuable metals from low-grade ores. The results of extended tests indicated that the bacterium is capable of extracting appreciable amounts of copper and cobalt from ore and mineral samples when sulfur is available in a state that can be readily assimilated by the organisms. Under the conditions of these tests, this organism was not able to assimilate and oxidize the sulfur as it occurred in the ores and minerals. Ores containing copper minerals in the silicate, carbonate, and oxide forms, in the presence of elemental sulfur, were more susceptible to bacterial action than ores containing copper minerals in the sulfide form. Thiobacillus thiooxidans remained active on elemental sulfur in the presence of some of the ores which were tested, but could not tolerate others. Therefore, strains of the bacterium were progressively adjusted to increasing concentrations (0.5 to 10 grams) of the individual ores until they could remain active on 10-gram portions of all ores being tested.

Jan 1, 1961

By W. S. Sanner

Anthracite was used extensively as a fuel in iron metallurgy from 1840 to 1880. In 1874, 226 of the 680 blast furnaces in the United States were operating on anthracite and producing almost one-half of the Nation&apos;s pig iron. However, by 1890, railroad expansion, the development of western iron-ore reserves, and the growing use of coke decreased the importance of anthracite as a metallurgical fuel. As a result, the last blast furnace designed exclusively for anthracite use was built in 1891. Because of the increased energy requirements of our expanding national economy, the abnormally high demands during national emergencies, and the proximity of anthracite deposits to eastern steel-producing areas, interest has grown in again using anthracite in iron metallurgy. Estimates of anthracite reserves indicate a 300-yr. supply at a production rate of 30 million tons per year. These large reserves dictate the development of an adequate technology for the use of anthracite by the metallurgical industry.

Jan 1, 1961

By J. R. Nettle

The purpose of these studies by the Federal Bureau of Mines was to determine the feasibility of refining low-grade hafnium by an inert-gas-shielded molten-salt electrorefining technique to produce a hafnium metal meeting reactor specifications. The techniques were adapted from those used success-fully for titanium electrorefining. Three electrolytes containing hafnium chlorides were developed from which deposits having a Brinell hardness of 170 or below were recovered. A KC1 + NaC1 + HfC14 electrolyte produced deposits in the hardness range of 140 to 165 Brinell. Deposits with a hardness range of from 132 to 152 Brinell were pro-duced from an electrolyte composed of KC1 + LiC1 + HfC14. A third electrolyte composed of NaC1 + K3HfC17 produced deposits with a hardness as low as 139 Brinell. In a fourth electrolyte, composed of NaC1 + K2HfF6, a measure of refining was accomplished, but under the test conditions no metal meeting specifications was recovered; none was softer than 174 Brinell. A number of metallic impurities were reduced in quantity by the electro-refining process, notably iron, which normally was reduced from 250 p.p.m. to less than 50 p.p.m. Magnesium generally was reduced from 680 p.p.m. to less than 80 p.p.m. Manganese content was also reduced by the electrorefining process. Sponge containing 90 p.p.m. Mn yielded deposits containing a maximum of 50 p.p.m.; some deposits contained only 10 p.p.m.

Jan 1, 1961

By R. J. Leary

Iron and steel scrap has accounted for 45 to 50 percent of the metallics used by the steel industry. In an electric furnace which utilizes a 100-percent cold charge consisting of about 99 percent scrap and 1 percent pig iron, sensible heat from molten pig iron is not present as it is when hot metal is charged to open hearths and converters. A study of means for more efficient utilization of iron and steel scrap in steelmaking indicated that the time and fuel requirements to melt scrap were important cost factors, particularly in arc-furnace steelmaking. A process to preheat scrap economically prior to charging into the arc furnace has been developed, utilizing efficiently the heat from combustion of fossil fuels as a substitute for electric-arc heating in the initial stage of arc-furnace steelmaking. Scrap is loaded into a portable vertical cylindrical furnace body that is open at the top and has a perforated dropout door at the bottom. In the heating operation, the furnace body containing scrap is placed upon a hollow base connected to a flue, and then the burner and combustion-chamber unit is lowered on top of the furnace body. The stream of hot-combustion products flows down through the bed of scrap imparting heat to it, and the cooled gases exhaust through the flue. After the heating operation the furnace body containing hot scrap is transported to the arc furnace for charging. Thus, the furnace body serves as a charging bucket for top-charged arc furnaces, enabling this preheating process to be integrated into existing material-handling patterns in many arc-furnace plants.

Jan 1, 1961

By H. E. Peterson

Rhenium occurs in very small quantities (12).4 In order for the Federal Bureau of Mines to conduct an investigation of rhenium sources and methods of extraction, it was necessary to devise improved techniques for detecting and measuring minute quantities of the metal. A modification of the procedure of Malouf and White (46) was developed which can be used to detect rhenium in concentrations as small as 0.1 part per million and can be used to measure quantities of 1.0 part per million. It can be used for the analysis of siliceous and calcareous ores, of molybdenite concentrates, of fumes, of flue dusts, and of other metallurgical products. Development of the method involved devising an amine extraction procedure for separating rhenium from all interfering elements except tungsten and a selective distillation procedure for separating rhenium from tungsten. Adoption of these separation procedures permits use of large samples and precise determination of rhenium by colorimetric analysis of the thiocyanate complex of rhenium by means of a spectrophotometer.

Jan 1, 1961

By Joseph Grumer

An instrumented spherical vessel has been used for many years to study laminar combustion waves. Concurrent measurements of flame speed and pressure-rise rates have led to evaluations of burning velocities, the pressure dependence of the burning velocity, and the expansion ratios of the gases passing through the combustion wave. For the most part, these studies have involved flames initially at atmospheric or subatmospheric pressure. The old spherical vessel used by the Bureau of Mines was not designed for use at elevated pressures. Moreover, being made of wrought iron, it was susceptible enough to corrosion to prohibit its use with many combustible mixtures that figure in industrial research. In mid-1956, under sponsorship of the Office of Naval Research, the Bureau undertook the development of a stainless steel spherical vessel capable of withstanding explosions of gaseous mixtures at initial pressures as high as 20 atm. and initial temperatures as high as 250° C. The design called for a double array (cross) of closely spaced small windows for observation of the flame as it traversed the vessel and a piezoelectric transducer to measure concurrently pressure-rise rates. Because no commercial contractor was willing to bid on the construction of such a vessel, it was built at the Bureau&apos;s Bruceton machine shop.7

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 R. Barany

This report contains the results of experimental work conducted by the Bureau of Mines to obtain the heats of formation at 298.15° K. of analcite, dehydrated analcite, lawsonite, anorthite, hexagonal anorthite, and leonhardite. Thermodynamic data for these minerals have applications in ceramics, extractive metallurgy, and particularly in geochemistry. Except for data on anorthite, no previous similar data existed. The present results will be a substantial aid in deriving the temperature-pressure-equilibrium relationships among these minerals. The heats of formation were determined by solution calorimetry, with hydrofluoric acid as the reaction medium. The results were expressed both in terms of the constituent oxides and in terms of the constituent elements. The heat of formation data were combined with related entropy values to obtain the free energies of formation at 298.15° K.

Jan 1, 1962

By K. K. Kelley

Thermodynamics data for silicates have applications in the fields of extractive metallurgy, ceramics, and geochemistry. To facilitate these applications, up-to-date tables of heats and free energies of formation are needed. It is the purpose of this report to supply such tables for anhydrous silicates. During the last 15 years the heats of formation of a substantial number of anhydrous silicates have been reliably determined at or near room temperature. This resulted from the development (first by the Bureau of Mines and later by the Geophysical Laboratory of the Carnegie Institution of Washington, by the Institute of Geology of the University of Helsinki, Finland, and by the Department of Geology of the University of Chicago) of accurate solution calorimeters, employing hydrofluoric acid as the reaction medium. Specific references to work of these laboratories will be made in the next section of this report. Also, entropy data at 298.150 K. and high-temperature heat-content values are available for many of these silicates, mainly owing to work of the Bureau of Mines. Most of these entropy and heat-content data have been compiled in Bureau of Mines Bulletins (13, 15).3

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 J. J. Wallace

This report describes the initial phase of Bureau of Mines research in the hydraulic mining of bituminous coal. The mining site and equipment are described, and the test procedures and results obtained with a bar-mounted monitor are given. Tests showed that hard Pittsburgh-bed coal can be mined hydraulically from a solid face at water pressures of 4,000 pounds per square inch.4 Coal was penetrated to a depth of 4 feet in 20 seconds with 225 gallons of water per minute coming from a 3/8-inch nozzle at 4,000 pounds per square inch pressure. Some difficulty was encountered in cutting the binders occurring in the coal; it was not possible Lu penetrate directly the overlying draw slate.

Jan 1, 1961

By S. R. Borrowman

This investigation by the Bureau of Mines was undertaken to develop information on the extractive metallurgy of thorite ores because potential ore bodies of this mineral have been found recently in Colorado, Idaho, and Montana. Basic information on thorite ore treatment that would be useful in appraising the potential of these and other domestic thorium resources was developed. The work was done mainly on thorite ore containing 3.87 percent ThO2 from the Powderhorn district, Colo., and on a composite sample containing 0.52 percent ThO2 from the Wet Mountains district, Colo. Limited tests of d corroborative nature subsequently were made on a sample containing 2.30 percent ThO2 from the Lemhi Pass area on the Idaho-Montana border.

Jan 1, 1962

By M. I. Copeland

The investigation of the iron-gadolinium phase diagram is part of a project undertaken by the Bureau of Mines and sponsored by the Atomic Energy Commission to investigate rare-earth alloys. Data from the investigation of the iron-gadolinium phase diagram revealed a single eutectic system with very limited terminal solubility and three intermediate phases. The eutectic point occurs at about 85 percent gadolinium, and the eutectic isotherm, which occurs at 850° C., extends from the compound Fe2Gd to 99-plus percent gadolinium. Very little solubility of the solid phases in each other was observed. The three intermediate phases, FegGd, Fe3Gd, and FeaGd, melt incongruently at peritectic isotherms at 1,320°, 1,150°, and 1,080° C., respectively. The crystalline systems of the three phases were determined as follows: FegGd, hexagonal; Fe3Gd, hexagonal or rhombohedral; and FeaGd, face-centered cubic. No lowering or raising of the alpha-gamma iron transformation at 910° C., the gamma-delta iron transformation at 1,388° C., or the gadolinium transformation at 1,262° C. was observed. The principal methods used in determining the iron-gadolinium phase diagram were melting-point determinations, thermal analyses, metallographic examination, and X-ray diffraction analyses. Melting, heat treating, and thermal analyses were conducted in a vacuum or under a helium atmosphere because of the avidity with which oxygen combines with gadolinium at elevated temperatures. A few hardness values were determined, but they had no part in the derivation of the phase diagram. No other mechanical properties were determined.

Jan 1, 1962

By C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

Jan 1, 1962

By A. A. Berk

The Bureau of Mines devised a test nipple for the field study of corrosion in the condensate-return lines of Federal heating plants. Corrosion surveys, made with this device, showed that the deterioration of the piping was caused principally by carbonic acid in the steam condensate. Corrosion problems were brought under control when the carbonic acid concentration in the condensate was decreased. In many instances, this was effected by decreasing the total carbon dioxide content of the feedwater; in others, the condensate acidity was neutralized with volatile, alkaline chemicals. Filming treatment with octadecylamine, reported successful in controlling return-line corrosion in industry, was much less effective in Federal area-heating plants. Laboratory study by the Bureau disclosed that octadecylamine is unstable in heating systems. Analytical methods were developed for this chemical and its degradation products in heating-plant condensate. Field surveys, in using these methods, confirmed the instability of the filming material. Laboratory tests showed that the degradation products are not useful film formers. Since filming treatment has little effect on condensate corrosivity, the piping was corroded where it was not coated by the treatment chemical.

Jan 1, 1962

By T. T. Campbell

This investigation was undertaken by the Bureau of Mines to determine if high-purity ductile molybdenum of uniform quality can be prepared by bomb reduction techniques. Molybdenum trioxide (Mo03) and mixtures of molybdenum dioxide (Mo02) and trioxide were reduced by magnesium in closed steel bomb reactors. Very high pressures in excess of 5,000 p.s.i. developed during magnesium reductions of Mo03. The addition of calcium oxide to the bomb charges caused a significant reduction in pressure. Reaction efficiencies higher than 95 percent were obtained during magnesium reductions of either Mo03 or mixtures of Mo02 and Mo03, but high pressures were encountered when the charges contained from 30 to 60 percent Mo02. Reaction efficiencies were usually low (less than 80 percent) when the bomb charges contained more than 40 percent Mo02. The charges with the best composition considering operating pressure, yield, and purity contained from 10 to 30 percent Mo02. The addition of small amounts of carbon to the reaction charges was helpful because some deoxidation occurred during the reduction and also during subsequent arc-melting of the regulus metal. The purity of the bomb-reduced, arc-cast molybdenum metal ranged from 99.2 to 99.8 percent and in some instances the metal contained as little as 5 parts per million oxygen.

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