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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 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 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 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

By N. E. Hanna

An investigation was made of pressure pulses produced by unconfined explosive blasts in underground openings. Four tests were made with TNT or modified amatol charges ranging in weight from 60 to 2,000 pounds; each test involved either single or multiple charges. Pressure-time profiles were obtained using mechanical self-recording pressure gages. The cube-root scaling law for peak pressure was found to be valid within about 1 tunnel diameter; at greater distances, the pressures obtained along direct paths were generally higher than this scaling law would indicate.

Jan 1, 1968

By Eldon C. Pattee

Reconnaisance samples of reported beryllium occurrences in Idaho, Washington, Montana, and Oregon were chemically and spectroscopically tested in a mobile laboratory. The two predominant types of occurrences were green beryl associated with Cretaceous intrusions and disseminated aquamarine associated with Tertiary intrusions. Although the beryllium content of known deposits in the Northwest is too low for economic development at present, total submarginal-grade beryllium resources in pegmatites are estimated to be 570,000 to 1,870,000 tons containing 0.024 to 0.167 BeO. A potential source of 500,000 to 700,000 tons of beryllium-bearing tactite in Idaho and Montana averages 0.033 to 0.080 percent BeO.

Jan 1, 1968

By F. W. Wood

The use of consumable.-electrode arc melting as a production technology is growing. One advantageous feature of this process is that it avoids ingot contamination by soluble crucible materials by employing a chilled metal crucible. Because the thermal balance under these conditions is rather delicate and does not necessarily provide a favorable environment for solidification, catastrophic imbalances can occur. The effectiveness and mechanistic roles of various factors are mostly unknown, and more intelligent insight regarding the distribution of temperature and heat is needed. Experience has provided several pertinent observations, some of which are quite superficial. The most meaningful data have resulted from studies of molten pool shapes and sizes and from measurements of heat flow through crucible walls. Overall experience, intuitively interpreted and supplemented, is sufficient nevertheless as a basis for a boundary-value treatment of the problem. A mathematical analysis based on a separation of variables, using conventional differential equation methods, provides a useful solution. For a cylindrical ingot, the temperature varies as a Bessel function of an argument proportional to the radius and as an exponential function of longitudinal position. Trial calculations using the problem solution seem to verify the general correctness of the result as compared with experience. The role and nature of solution parameters are also clarified, though not entirely resolved. It is revealed that the barrier to heat flow at the ingot-crucible surface has a prominent influence. Utility of the model embodied in the problem solution is readily demonstrated by considering a variety of contemporary questions about arc melting, and it is hoped that utility can be enhanced by improvement of the model.

Jan 1, 1968

By Robert A. Bradburn

The Bureau of Mines has developed a miniature, portable two-level oxygen-deficiency alarm and produced three prototype models. Each operates from a 4.2-v dc power source, and the highest current drain of any model is 80 ma. An electrochemical cell, which produces an electrical output in proportion to the partial pressure of oxygen to which it is exposed, is used as an oxygen detector. The output of the cell is applied to an electronic circuit that detects two different levels of oxygen percentage below that of normal air, and produces distinct audible signals at these levels. The hazard alarm mode is activated when the oxygen percentage first drops below normal and produces a 500-cps "beep" tone with an intermittency of 1 cps. The danger mode produces a continuous 500-cps audible signal when the oxygen percentage drops still lower.

Jan 1, 1968

By Martin H. Stanczyk

Bench scale, laboratory batch attrition grinding tests were made of a coarse commercial kaolin in a stainless steel, 5-inch-diameter attrition grinding machine to study the effect of a number of basic operating variables on particle size reduction and electric energy consumption. The results of the investigation showed that the more important operating variables influencing the efficiency of kaolin comminution and energy consumption requirements were type, size, and shape of grinding media, grinding media to clay weight ratio, peripheral rotor speed, clay slip pulp density, degree of pulp dispersion, and the angular arrangement of the rotor and stator bars. The tests also indicated that variables having less influence on grinding efficiency and energy consumption were pulp temperature, design of rotor cage, rotor clearance, rotor-stator bar interval, addition agents, pulp level, degree of pulp aeration, and chamber liners. The research showed that grinding media had the greatest influence on abrasion of machine parts and that spherical-shaped grinding media were superior to sharp angular or long bladed media with respect to media degradation, machine abrasion as well as grinding efficiency.

Jan 1, 1968

By W. L. Acherman

The Bureau of Mines found the chemical and galvanic corrosion behavior of the TZM and molybdenum-30 tungsten alloys to be generally equal or superior to that of unalloyed molybdenum in many aqueous solutions of acids, bases, and salts. Notable exceptions occurred in 1 [N] nitric acid, where both alloys corroded appreciably faster than molybdenum. In mercuric chloride solutions, the TZM alloy was susceptible to a type of crevice corrosion which was not due to differential aeration. The alloys were usually not adversely affected by con-tact with dissimilar metals in galvanic couple experiments, but the dissimilar metals sometimes corroded galvanically. Both alloys were resistant to substitute ocean water spray at 60° C.

Jan 1, 1968