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By Oliver C. Fursman

The Bureau of Mines undertook this investigation in order to determine the feasibility of producing commercially acceptable alumina and iron by application of the Pedersen process to high-silica, high-titania, ferruginous bauxites of the Pacific Northwest. Calcium aluminate slags were produced by smelting bauxite with coke and lime in an electric-arc furnace. Over 90 percent of the total alumina can be extracted by sodium carbonate solution from slags of properly controlled ternary-phase composition (CaO-Al203-SiO2) that are cooled slowly enough to permit adequate crystallization of the 2CaO-SiO2 and the calcium aluminate compounds. Most of the iron charged was recovered in the regulus; the slag contained about 2 percent iron (as iron oxide), regardless of smelting time.

Jan 1, 1968

By T. N. Rushton

Rate minima are encountered in the reduction of magnetite with hydrogen. In a certain temperature zone, the reaction rate decreases with rise in temperature. This is inexplicable by classical kinetic theories; neither is a transition in reduction mechanism suitable for interpreting the observed behavior, This anomaly can be fully explained by hypothesizing two species of chemisorbed hydrogen with different adsorption coefficients and activation energies for adsorption. Competition between two energetic states of adsorption occurs with temperature rise, with the low energy state predominating below the anomalous temperature zone and the high energy state above it. The presence of two possible adsorption sites appears to be characteristic for oxidic adsorbents.

Jan 1, 1968

By Wesley T. Holmes

This report describes the first phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected slag compositions in the titania-alumina-silica-calcia-magnesia system. Both the melting-holding-quenching method and the hot-stage microscope method were used in the tests. Liquidus temperatures of slags studied ranged from 1,217° to 1,667° C. The lowest liquidus temperature of the slags occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. Liquidus temperatures were also lowered when Si02 was substituted for Ti02 plus Al2O3 when CaO and MgO levels were held constant. Improved methods for the measurement of liquidus temperatures on very small samples are described.

Jan 1, 1968

By T. A. Sullivan

Refining in a molten salt electrolyte was investigated as a means of recovering nickel containing less than 1 percent and preferably less than 0.2 percent cobalt from nickel products containing up to 5 percent cobalt. Electrolytic separation of nick and cobalt was accomplished in a molten KCl-LiCl-NiCl2 electrolyte. Nickel containing less than 0.10 percent cobalt was routinely prepared. Factors that influenced the transfer of cobalt to the refined product were the nickel concentration of the electrolyte, the cobalt concentration of the electrolyte, the ratio of nickel to cobalt in the electrolyte, and cathode current densities. A method of recovering the cobalt from the electrolyte was developed. The possibility of preparing high-purity nickel by this process was shown, as well as the preparation of various cobalt-nickel-tungsten alloys.

Jan 1, 1968

By Wesley T. Holmes

This report describes the second phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected synthetic slag compositions in the Ti02 -A1203 -FeO-Si02 -CaO-MgO system. Both the hot-stage microscope and the strip furnace (melting-holding-quenching technique) were used during test procedure to determine the effects of CaO, MgO, and SiO2 on the liquidus temperature of slags. The liquidus temperatures of slags studied ranged from 1,241° to 1,900° C. The lowest liquidus temperature for each Ti02 plus A1203 plus FeO weight-percent generally occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. In this investigation substitution of either CaO or MgO for SiO2 and MgO for CaO raised the liquidus temperature of more than 50 percent of the reported base slags when Ti02, A1203, and FeO contents were held constant. The results of this investigation may serve as guidelines for determining flux requirements in smelting a wide variety of titaniferous magnetite concentrates or ores.

Jan 1, 1968

By R. G. Peluso

Methods and results of studies to determine friction and shock losses encountered in auxiliary face ventilation systems utilizing flexible, spiral-reinforced ventilation tubing are presented. The results, tabulated in graphic form, simplify fan selection and enable mine operators to design adequate auxiliary ventilation systems. Problem illustrates the use of graphs.

Jan 1, 1968

By Edward W. Parsons

The transverse force developed by expansion-shell rock-bolt anchors on the wall of a drill hole as the bolt is tensioned was measured by the Bureau of Mines using a device specially designed and fabricated for attachment to a universal testing machine. Load cells equipped with electrical-resistance strain gages provided the data from which the transverse force, in pounds, was calculated. Seven different expansion-shell anchors were tested, and the ratio of transverse force to bolt-tension load was found to range between 0.98 and 1.94 to 1.0. The drag load appeared to be the major cause of the transverse-force variation, but the relative effects of individual factors that affected the ratio between the transverse force and the bolt tension were not determined.

Jan 1, 1968

By R. L. de Beauchamp

A preliminary investigation was made of the extraction of chromium from ferrochromium by low-temperature chlorination in the 3400 to 5250 C range. The objective was to devise a method for separating chromium from iron in high-carbon ferrochromium produced from domestic chromite concentrates. The majority of iron was removed as a volatile chloride; chromium was contained in the residue as a nonvolatile chloride, which was separated from carbon and unattacked ferrochromium by dissolution. A small rotary chlorination apparatus was designed, built, and used for the chlorination tests, and samples of commercial-grade high-and low-carbon ferrochromiums were chlorinated for comparison of chlorination characteristics. Low-temperature chlorination of three types of ferrochromium resulted in the removal of 81.9 to 91.6 percent of the iron content as sublimed FeC13. Recovery of chromium in a leach solution of the reactor product varied from 82.4 to 93.1 percent.

Jan 1, 1968

By Manuel Gomez

Coking time was investigated as a function of coal properties, carbonization parameters, and the interactions between these variables. The results indicate that coal properties and carbonization conditions interact to influence the coking time, and these interactions may be determined quantitatively. Prediction equations were developed and used to simulate the effects of bulk density, flue temperature, and oven width on coking times for coals having a wide range of properties. The data presented provide additional information on the carbonization process to permit the coke oven operator to maintain closer control of coke production and coke uniformity.

Jan 1, 1968

By Wilbert T. Malenka

A modified factorial experiment was used to determine the effect of operating factors in hydraulic mining of anthracite. Seven basic factors at various levels were considered. The significant factors were found to be pressure-volume, pattern, and jet traverse speed. Mining data were programed for computer, and a prediction equation was determined from printout information based on the hydraulic "jumbo" operating parameters and characteristics of anthracite, The source of error is discussed. The prediction equation is general in nature and might be useful in delineating performance characteristics in the design of equipment and/or more effective utilization in a medium with characteristics similar to those of anthracite.

Jan 1, 1968

By D. J. Bauer

Oxidation of mixed lanthanide solutions with ozone at pH 4.5 and at ambient temperature resulted in precipitation of 98 percent of the original cerium present. Corresponding cerium purity was increased from 50 to 98 percent. A second ozone oxidation-precipitation step produced cerium of 99.9 percent purity in high yield from the 98-percent-pure material. Alternately, ozonation at pH 6.5 and 85° C differentially precipitated cerium and rare-earth elements heavier than cerium and left 89 percent of the original lanthanum in solution at a purity of 95 percent. Subsequent recovery of cerium from the heavier rare-earth elements in the precipitate was accomplished by dissolving the precipitate in dilute mineral acid and reoxidizing the cerium with ozone at pH 4.5 and at ambient temperature. The filtrate contained an enriched praseodymium-neodymium-samarium-europium mixture that is amenable to separation by ion exchange or solvent extraction.

Jan 1, 1968

By Ronald P. Hollenbeck

Shales in the Appalachian Region of Kentucky and Tennessee were sampled and tested to determine their use as raw materials for the manufacture of lightweight aggregate by the rotary-kiln method. Nine samples were obtained from eastern Kentucky and 143 samples were obtained from eastern Tennessee. As a result of preliminary testing of these samples, two sources in eastern Kentucky and 11 sources in eastern Tennessee were resampled for rotary-kiln tests. The rotary-kiln tests showed the two sources in Kentucky and seven sources in Tennessee contained shale that would produce satisfactory aggregate. Lightweight aggregate processed from these nine sources was tested in concrete shapes and was found to be suitable for use in structural concrete.

Jan 1, 1968

By A. G. Starliper

The Bureau of Mines made laboratory investigations to determine the feasibility of utilizing fine tungsten wires to reinforce a number of nonferrous metals and alloys and a superalloy, S-8l6. The composites of tungsten filament and metals were chosen to attain elevated temperature strength and corrosion resistance. Oriented clean or precoated tungsten wires were incorporated with the other metals by extrusion, swaging, and infiltration casting. Although widely varying characteristics were found in the composites, none were considered satisfactory for high-temperature use, chiefly because of reactions between the matrix metal-tungsten surface. Diffusion, solution, and chemical reactions between matrix and tungsten wires were sufficiently slow for some combinations, such as 15 v/o 8-816, to exhibit increased high-temperature strength for a limited time. A few metals failed to wet or bond to the tungsten surfaces, while a few responded after precoating with a third metal.

Jan 1, 1968

By R. P. Adams

Because of the extreme interest in materials with high melting temperatures and the advantages offered over the powder route for making high-density material, arc-melting and centrifugal-casting methods were investigated for preparing shapes of hafnium carbide with and without excess carbon. Highly satisfactory equipment was constructed and efficient operating procedures were established. Also, methods for preparing consumable electrodes and shrink-tolerant graphite molds were developed. Although crack-free hafnium carbide (6.3 weight-percent carbon) shapes were not made, coherent castings containing 9 to 13.5 weight-percent carbon were produced; the same compositions were shown to be resistant to thermal shock. Selected physical and chemical tests were performed on castings chosen for investigation by chemical and nondestructive inspection techniques. Electrical conductivity and thermal expansion measurements were made. Measurable oxidation of all the compositions studied was observed to start between 500° and 600° C. Attack by nitrogen, however, did not occur until temperatures exceeded 2,000° C. A linear relationship of the logarithm of the diamond pyramid hardness to the temperature was noted. Considerable scatter of the bend-rupture strengths at room temperature and of the tensile strengths up to 2,000° C was found. However, at the latter temperature and above, a definite relationship of strength to temperature was observed and some ductility was noted.

Jan 1, 1968

By A. F. Colombo

Bench-scale research was undertaken to determine if adding ammonia to cyanide leaching solutions would enhance the extraction of copper from an argillaceous Michigan copper ore. Two leaching techniques, (1) rolling using a tumbling bottle and (2) aerating using a modified Buchner funnel, and variations in pulp temperature; were employed in evaluating the effect of ammonia concentration on copper extraction. Under these experimental conditions, the extraction of copper was shown to be independent of ammonia concentration and entirely dependent on cyanide concentration.

Jan 1, 1968

By E. L. Litchfield

The electrification of ammonium nitrate-fuel oil (AN-FO) blasting agents by pneumatic loaders is described and discussed. The consequences of the electrification are considered in light of the initiation requirements of electric blasting caps. It is recommended (1) that semiconductive loading tubing be utilized and (2) that the resistivity of the AN-FO be controlled; it is further recommended that the operator (3) test to assure continuity of the electric detonator legwire-bridgewire-legwire circuit prior to insertion of the cap into charge or borehole, (4) keep the legwires shunted but not otherwise connected to ground during loading of the blasting agent into the borehole, (5) assure that the borehole is discharged prior to hooking up the detonator leads, (6) assure that he is himself discharged prior to handling the detonator leads, and (7) assure that the blasting cap leads are never carried to the AN-FO loader. The basis and significance of these recommendations are explained.

Jan 1, 1968

By Philip C. Good

Red mud residue from Bayer process treatment of Jamaican bauxite was dewatered in batch and in continuous centrifuges. Solids content of the residue was increased from its original value of 20 to 25 percent to about 40 percent by centrifuging. Clear effluent amounting to approximately 40 percent of the slurry liquid was recovered containing dissolved alumina and soda values for potential recycle to the alumina plant" Addition of a chemical flocculant to the centrifuge increased capacity by about 35 percent. Manufacturer's estimate of large-scale equipment requirements, based on data collected in this investigation, was that a proposed installation for dewatering 16,000 tons per day of Jamaican red mud would require twenty-two 24-by 60-inch solid-bowl-type centrifuges. Cost analysis of a proposed installation, based on a Jamaican red mud tonnage of 16,000 per day, is included also.

Jan 1, 1968

By Manuel Gomez

Bituminous coals having maximum fluidity values in the 40- to 25,400-dial-divisions-per-minute (ddpm) range were carbonized in a continuous, entrained-bed reactor. Carbonization was conducted in an 8-inch diameter, vertical reactor at temperatures from 955° to 1,345° F and at air-to-coal ratios ranging from 4.63 to 16.12 scf/lb of moisture-and ash-free coal charged. Carbonization rates from about 118 to 360 lb/hr, as-carbonized basis, were examined. It was demonstrated that carbonization temperature and air-to-coal ratio must exceed minimum values for continuous operation. Within the operating conditions discussed, highly fluid bituminous coal was carbonized to produce tar and nonagglomerated char. The yield of tar ranged from 21.3 to 38.9 gallons per ton and the char yield ranged from 1,109 to 1,563 pounds per ton, all units expressed on a moisture-and ash-free basis. It was demonstrated that the maximum fluidity and the average size of the coal along with the air-to-coal ratio and the carbonization temperature act together to influence the carbonization product yields and certain properties of the products. Prediction equations were developed from the data for product yields and selected properties of the char, tar, and gas.

Jan 1, 1968

By P. M. Johnson

A design for a laser-powered optical interferometer, using a specimen whose thermal expansion is to be measured as part of the optical system, was conceived and applied in a prototype dilatometer. The object of thin work was the development of an absolute dilatometer capable of use at elevated temperature, particularly above 1,000° C. The prototype has been operated at temperatures exceeding 1,510° C. Results obtained with this device agree within 2.5 percent with the published data for the coefficient of expansion of columbium.

Jan 1, 1968

By M. J. Ferrante

The preparation and subsequent reduction of vanadium trichloride was investigated as a process for the production of high-purity vanadium metal. Chlorine was reacted with vanadium oxide in the presence of carbon to vanadium tetrachloride. The contaminant vanadium oxytrichloride was also formed and later converted to tetrachloride by reaction with chlorine in the presence of activated charcoal. Vanadium tetrachloride was stirred continuously during thermal dissociation to vanadium trichloride powder from which volatile contaminants were removed by distillation. The vanadium trichloride powder was reduced to vanadium sponge by controlled feeding of the trichloride into molten magnesium. Excess reductant and byproduct salt were removed from the vanadium sponge by high-vacuum distillation. Batches as large as 6.5 kilograms of sponge metal were prepared at an average reaction efficiency of 98 percent. Vanadium sponge after consolidation by arc-melting contained 820 to 11330 ppm of interstitial impurities and had a hardness between Rockwell B 40 and 70, This metal exhibited excellent workability at room temperature. The purification of impure vanadium metal by electron-beam melting resulted in lowering interstitial impurities from 1,890 to 504 ppm and hardness from Rockwell B 87 to 28.

Jan 1, 1968