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By D. E. Kirby

The electrochemical reduction of AlC13 was investigated as a process for the production of aluminum. An externally heated, single-compartment cell with a rammed refractory lining was used with molten KCl-NaCl-AlC13 electrolyte. Aluminum was deposited qt 700° to 760° C with a current of 100 to 200 amperes on a molten aluminum cathode. Chlorine was evolved at a graphite anode and collected and measured to provide a quantitative evaluation of the AlC13 reduction. Aluminum was removed from the cell by siphoning or ladling. Granular AlC13 was added periodically to replenish that depleted from the electrolyte. Concentrations of 7.5 to 17.5 percent AlC13 in the electrolyte were optimum for operation. Anode current efficiencies of 83 to 85 percent were attained, using anode current densities of 5.9 amperes per square inch and an anode-cathode distance of 4 inches. The chemically bonded, alumina liner was resistant to attack by aluminum and chlorine but susceptible to erosion at the surface of the electrolyte. Titanium diboride proved suitable for the electrical connection to the molten aluminum cathode. Aluminum of a purity equal to or better than 1100 series metal was electrowon continuously from commercial AlC13 for a period of 4-1/2 months.

Jan 1, 1970

By N. N. Moebs

The Bureau of Mines air-sealed a 77-acre) above-drainage coal mine to evaluate sealing as a means of reducing the acid and metallic salt contents in drainage from abandoned mines. An approximate reduction in acidity of 150 ppm (equivalent to 193 pounds per day) and in iron of 98 ppm were directly attributed to sealing. The topographical, hydrological, and other factors involved in air-sealing are discussed, and the construction used to seal the mine is described.

Jan 1, 1970

By Richard A. Dick

Underground blasting in permanently frozen gravel was studied in a 7-by 12-ft drift by running a nonreplicated 2 X 2 X 2 factorial experiment on the effects of type of cut, delay, and explosive on the fragmentation subsystem. Comparisons were made between a V-cut round and a burn-cut round, millisecond delays and half-second delays, and 40 percent special gelatin and 60 percent high-density ammonia dynamite. The number of large blocks in the muck pile) loading time, shuttle car operating time lost because of cleanup needs, length of advance per round, and length of muck pile were recorded and statistically analyzed. None of the blast parameters had a significant effect on the length of advance or length of muck pile, although the half-second delays tended to give a shorter muck pile than millisecond delays. The burn cut required less secondary breakage, less loading and cleanup time, and gave better overall fragmentation than the V-cut. The ammonia dynamite shots required less secondary breakage and less loading time than those using special gelatin. The half-second delays gave better overall fragmentation and required less cleanup time, but the millisecond delays gave a better loading rate. None of the differences between delays and explosives were notably significant.

Jan 1, 1970

By Laurence G. Trudell

A geologic framework for interpreting stratigraphic and geographic variations of the Green River Formation in the Piceance Creek Basin is developed from lithologic data accumulated by the Bureau of Mines from oil-shale coreholes. From detailed Bureau of Mines descriptions of samples from nine coreholes and supplementary lithologic data from seven additional sampled sections, three cross sections were constructed along lines transecting the basin. Plotted as lithologic columns with corresponding oil yields and resistivity logs, the sampled sections are correlated on a time-stratigraphic basis. Distribution and correlation of nahcolite and halite zones are shown, and the approximate base of leaching of these saline minerals is indicated. General lithologic characteristics of members and zones are discussed and interpreted. Large-scale lithologic logs illustrate the nine Bureau of Mines core descriptions, and the complete description of Bureau of Mines-Atomic Energy Commission Colorado Corehole No. 1 is included in an appendix. The time-correlated cross sections provide a necessary framework for understanding the depositional history of the Green River Formation and will facilitate evaluation of oil shale and other mineral resources in the Piceance Creek Basin.

Jan 1, 1970

By D. Bienstock

A rig was constructed to burn 100 to 125 lb of coal per hour at 4,000° F in a cyclone burner with oxygen-enriched air preheated to 1,500° F to ascertain the problems in the coal-fired MHD generation of power. Potassium carbonate was added to the coal at several concentrations up to 1.23 g-moles/kg of coal (17 lb K2C03/100 lb coal). Boiler-tube materials maintained at wall temperatures of 800° to 1,500° F were exposed to the combustion effluent of 1,800° to 2,500° F. Practically complete removal of sulfur dioxide from the stack gas was achieved with the seed addition. Nitric oxide formation followed theoretical expectations at combustion temperatures with some decomposition of the NO occurring as the gas cooled flowing through the system. Nitrates in the fly ash were less than 1.7 percent of the total fixed nitrogen. With aqueous extraction of the fly ash a maximum recovery of 75 percent of the potassium was obtained. Haynes 25 was unattacked at a wall temperature of 1,500° F in combustion gas at 2,500° F; the stainless steels 310, 316, and 446 were resist-ant at a metal temperature of 1,100° F in gas at 2,100° F.

Jan 1, 1970

By L. A. Neumeier

The Bureau of Mines evaluated the properties and anisotropy in properties of rolled Zn-Cu and Zn-0.12 pct Ti-Cu alloys with various copper additions to 1.25 pct. The alloys were rolled cold and at various hot-rolling temperatures to reductions as high as 92 pct after breakdown rolling. The properties are extremely sensitive to various combinations of composition, rolling temperature, and rolling reduction, Zn-Cu alloys can develop good creep resistance, but they are inferior in that respect to Zn-Ti-Cu alloys. For alloys either with or without the titanium addition, cold-rolling results in recrystallization of the matrix and rejection of copper from solution, causing poor hardness, tensile, and creep properties, but high ductility. Peak tensile strengths develop when the alloys are rolled in the range 320° to 400° F, Best creep resistance for Zn-Cu alloys requires higher rolling temperatures when copper content is increased. Creep resistance is best for Zn-Ti-Cu alloys with about 0.75 to 1.0 pct CU rolled near 480° F. Some copper is soluble in the TiZn15 phase, which forms into "stringers" during rolling. The possible contributions to creep behavior of factors such as distribution of second-phase particles, grain size, and preferred orientation are discussed.

Jan 1, 1970

By V. A. Cammarota

In this report, the effects of anode-production variables, such as aggregate coke sizes, pitch binder content, and baking cycle, were investigated. A small alumina reduction cell proved effective in evaluating anodes prepared from commercial materials and from lignite coke and pitch. Compressive strength was found to be the physical property most significantly influenced, but it did not appear to affect anode consumption. Specific carbon consumption, that is, the ratio of carbon in the anodic gas to carbon theoretically oxidized at the anode, was used as an index of anode consumption. It was found that an anode made with lignite coke and commercial pitch was very low in consumption; however, anodes made completely from lignite but by a different fabrication method showed high consumption and anode deterioration. Microscopic examination of anodes after electrolysis showed evidence of higher consumption at low current densities, and was useful in judging overall anode quality. Based on the physical properties of the anodes and their consumption during electrolysis, lignite can be a suitable material for anodes, provided the proper fabrication conditions are used.

Jan 1, 1970

By Robert M. Doerr

The research objective was to determine the effect of vanadium alloy additions on the oxidation behavior of cobalt-nickel Alloys. Eighteen alloys were reacted with 0 2 at 0.5 arm and 1,351°, 1,389°, and 1,429° K. The alloy compositions consisted of Co-Ni master alloys (0, 22, 50, 70, 91, and 100 wt pct Ni) with V additions of 0, 0.9, and 2.7 wt pct. Large early deviations from, or changes in, the parabolic rate constant were encountered, but the reaction rate in most cases declined approximately in accordance with the parabolic rate law. Relatively, the vanadium degraded the oxidation resistance most at the highest nickel contents. In some cases, melting of the oxide was inferred from microscopic evidence and X-ray diffraction measurements disclosed the presence of low-melting vanadates.

Jan 1, 1970

By R. Newman

An inexpensive slow-speed data acquisition system has been adapted to digitally record multiple parameters simultaneously at intervals of 15 seconds. The system was built for use with standard soils testing equipment to automatically record load and displacement parameters at predetermined instants in time. Simultaneous readout is achieved by the use of special signal conditioner and sample-and-hold circuits which read the multiple signals simultaneously and hold them until the slow acting system can print out. Three channels of a 10-channel system have been converted and found to operate successfully during a series of direct shear tests. A unique feature of the system, which significantly reduced its cost, is the power supply units. Dummy circuits are used to maintain a constant power demand during sampling) thus eliminating the need for a costly power supply with rapid response characteristics. The entire system, having an overall accuracy of 0.25 percent, was put in operation for a cost under $2,500.

Jan 1, 1970

By J. Vance Batty

The Permian Red Bed copper deposits of the South Central States are a potentially important resource. Only the higher grade, near-surface ores are now exploited because conventional froth flotation does not recover oxidized copper minerals which comprise 10 to 15 percent or more of the copper content of typical ore. Laboratory-scale beneficiation studies were initiated to devise a method capable of recovering both sulfide and oxidized copper mineral. Testing established that the high clay and gypsum content of typical ore prevented effective flotation of the oxide mineral using sulfidizing, fatty-acid, or oil emulsion techniques. A modified leach-precipitation-flotation (L-P-F) procedure recovered over 90 percent of the copper, compared to a recovery of 77 percent obtained by conventional sulfide flotation. The higher costs of the L-P-F method would reduce the increased revenue from higher copper recovery. An increase in copper price and/or an increase in oxide copper content of the ore would make the L-P-F process comparatively more attractive.

Jan 1, 1970

By R. B. Tippin

To study continuous operation of the heavy liquid separation (HLS) of minerals, the Bureau of Mines concentrated spodumene from a typical ore. The studies included heavy liquid concentration, removal of the heavy liquid from the mineral products, and recovery of the heavy liquid for reuse. The research program examined the influence of feed moisture, steam consumption, stripping time, and condition of steam. Operation of multiple cyclones in series resulted in spodumene concentrates assaying 92 to 95 percent spodumene and indicated mineral recoveries of 86 to 89 percent. Continuous filtration and steam stripping produced mineral products containing less than I pound of heavy liquid tetrabromoethane (TBE) per ton of material. Problems unique to this process are discussed, including heavy liquid properties and viscosity, toxicity, material handling hazards, and safety precautions.

Jan 1, 1970

By James C. Patterson

Sintered fly ash was shown to have promise as a modifier for poorly drained soils. Turf grown in mixtures of sintered fly ash and soil benefited from increased water-infiltration rates, greater total pore space, and higher moisture availability, The result was an improved turf stand with increased grass yield and root density.

Jan 1, 1970

By Larman J. Heath

Wellbore enlargement was tested using hydrazine hydrate in a gas-storage well in Ohio to increase the well productivity. The wellbore was to be enlarged by chemical disaggregation of the sandstone adjacent to the wellbore. Productivity immediately declined 49.1 percent and gradually declined to zero in 7 months. A down-hole camera survey showed a white-to-gray precipitate covering the entire wellbore surface. The precipitate was chemically analyzed and identified as mostly carbazic acid, a hydrazine derivative of carbonic acid. Formation of this precipitate was not anticipated; this viscous sub-stance caused the gradual loss in productivity of the well. The wellbore was not enlarged. Laboratory tests were run to determine what clay stabilization measures could be taken in sandstone cores to prevent clay swelling and particle migration caused by hydrazine hydrate. Normal clay stabilization methods did not prevent the virtually complete loss in permeability to hydrazine hydrate. Other laboratory tests using natural gas diluted with small amounts of carbon dioxide confirmed the ease with which carbazic acid could be formed in a hydrazine hydrate-saturated environment within and adjacent to the wellbore.

Jan 1, 1970

By R. L. Blake

The crystal structure of hematite, a-Fe203, has been refined as part of a continuing study of the behavior of phases in the Fe-O system during reduction and oxidation. Three-dimensional diffraction intensities were collected on two spherical single crystals of hematite with a semiautomated Buerger single-crystal diffractometer. The first crystal refined was a natural Elba hematite with minor impurities. The other, a synthetic crystal, was refined at the request of Mossbauer spectroscopy investigators concerned with impurities in the natural crystal. The structure has been refined with a least-squares program and the final structure for the natural crystal irradiated with CuKa-radiation gave a discrepancy factor (R) of 3.65 percent using 49 unrejected reflections of the 51 measured. For the synthetic crystal, using MoKa-radiation, the discrepancy factor converged to 2.8 percent using 95 unrejected reflections and was 3.3 percent for all 109 reflections. The structure model of Pauling and Hendricks has been confirmed with essentially no change in the iron coordinates and approximately a 5-percent change in the oxygen coordinates. Selected interatomic distances and angles were calculated as were anisotropic temperature factors.

Jan 1, 1970

By G. H. Keith

Electrowon tungsten powders were investigated with respect to consolidation, fabrication, and mechanical properties. Sheet, 0.03 inch thick, was produced and its tensile strength measured between 250° and 1,935° C. The large particle size of electrowon tungsten effectively precluded sintering to a density sufficient to allow hot working to sheet or bar. The powders were consolidated by die pressing to 70-percent density, sheathing in molybdenum, and high-energy-rate extruding to either round or sheet bar of 100-percent density. The material was then rolled conventionally to sheet. The mechanical properties of the sheet prepared from the electrowon powders compared favorably with those reported in the literature for sheet prepared from commercially produced hydrogen-reduced powder.

Jan 1, 1970

By Daniel C. Boteler

Five lignites from the northern Great Plains province were carbonized at temperatures from 500° to 1,000° C in a bench-scale unit. A replicated Greco-Latin square experimental design was employed to allow testing of four independent variables at five levels. Independent variables investigated were temperature, source of lignite (mine), weight of charge, and moisture content of charge. Dependent variables were char yield, tar yield, light-oil yield, tar plus light-oil yield, carbonization gas yield, and carbonization gas heat yield. An analysis of variance indicated that, at the 99-percent confidence level, the independent variables of carbonization temperature, source of lignite, and weight of charge were significant for yields of char, tar plus light oil, and carbonization gas, whereas moisture content was only significant for carbonization gas yields. At the 95-percent confidence level, moisture content significantly influenced the carbonization gas heat yield per pound of lignite charge and the yields of dry tar plus light oil. All dependent variables were determined on a moisture- and ash-free basis. Multiple regression equations for predicting seven different factors of carbonization yields as functions of carbonization temperature and initial composition were developed using computer techniques. Equations for yields of char, tar plus light oil, and carbonization gas were compared with equations previously developed by others at the 500° C level.

Jan 1, 1970

By Joseph L. Condon

Fifteen shots of three explosives with charge weights of 0.52, 1.1, 3.1, and 5.1 kilograms were fired in a pond to study the seismic effects of detonating explosives in water. Shock pressures and bubble periods were measured with pressure transducers in the water. Vibrations were measured on land in three orthogonal directions with particle velocity gages. Statistical tests indicated that a charge weight exponent of 0.43 best scaled the data. While shock pressures and bubble periods showed considerable differences in explosive performances, the amplitudes of ground vibrations showed less difference, and one prediction equation was therefore derived to estimate vibration amplitudes from all the explosives.

Jan 1, 1970

By H. R. Babitzke

As part of a continuing project to develop refractory metal alloys for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation strengthening techniques to improve the properties of columbium alloys. The purpose was to investigate the effects of hafnium, tungsten, and boron on the formability, strength, and oxidation resistance of columbium. The experiment was of factorial design with two replications which called for 72 ingots of 36 basic compositions, weighing 150 grams each. Hafnium, tungsten, and boron were evaluated at 3, 3, and 4 levels, respectively. Values of alloy content are all in atomic percent. The highest strength observed was 29,000 psi at 1,200° C for alloys Cb-15Hf (No. 3), Cb-7.5Hf-5W-2B (No. 14), and Cb-15Hf-5W-2B (No. 15). At 1,200° C, the ternary alloy Cb-15Hf-5W (No. 6) which has shown good properties in previous Bureau of Mines investigations was the most resistant to oxidation For boron additions, the alloys oxidized more readily with increasing amounts of this element. The fabricability of the alloys high in boron became increasingly difficult, resulting in an inadequate number of alloys required for a complete statistical analysis for all the tests. As a result of the decrease in ductility, an insufficient quantity of tensile samples were available for a proper analysis for the high-temperature strength data.

Jan 1, 1970

By B. H. Eccleston

The effect upon automobile emissions in changing from leaded to lead-free gasolines was studied in experiments by the Bureau of Mines in cooperation with the American Petroleum Institute. Typical U.S. leaded gasolines and prototype lead-free gasolines of comparable octane quality were used in eight vehicles operated to simulate city driving. The experiments were run at 70° and 95° F. Exhaust and evaporative emissions were measured and the photochemical effect of the emissions was experimentally observed in an artificial smog chamber. Results of the study reveal the manner and degree in which the changes in fuel composition alter the amount and characteristics of both exhaust and evaporative emissions. Briefly, it is shown that the compositional differences between leaded and prototype lead-free fuels resulted in higher photo-chemical pollution potential of the emissions from the lead-free fuels. The effect is attributed to the photochemical characteristics of high-octane fuel components that are used in greater quantity in the lead-free fuels.

Jan 1, 1970

By W. R. Hardwick

Nuclear explosive fracturing has been suggested as a method to make hard rock amenable to extraction by a modified block-caving method. To evaluate this possibility, conventional and nuclear blasting practices are discussed, underground mining methods for large deposits and their costs are described, and the cost of fracturing ore with a nuclear explosive and subsequent mining by a modified caving system is estimated and compared with both open-stope and block-caving mining costs. While the direct cost of fracturing the ore in hard rock with a nuclear explosive is less than with conventional explosives, additional costs imposed by the use of nuclear explosives may make their use unattractive for deep mining.

Jan 1, 1970