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By D. A. Keefe, O&apos

The electrowinning of beryllium from beryllium oxide (BeO) using a molten-salt electrolyte composed of 56 LiF-37 BeF2-7 BeO (mole-percent) was investigated. Anodes made of porous carbon were found to be superior in current-carrying capacity and gave a lower cell voltage than other types of anode material tested. When porous carbon anodes were used) the resultant increase in anode area prevented anode passivation. The cell voltage was 3.3 volts) and electrode current efficiencies of 50 to 70 percent were obtained. The electrodeposited beryllium was recovered as beryllium powder or was coalesced to metal beads by heating to 1,300° C.

Jan 1, 1970

By Lester J. Crow

This study advances the use of elemental sulfur in structural materials by demonstrating its value in bonding high-strength, well-graded basalt aggregates to form sulfur-basalt concretes. Sulfur is an excellent bonding agent, and the strength of a thermoplastic sulfur-aggregate mixture depends, to a large degree, on the strength and grain-size distribution of the aggregate used. A 3-cubic-foot, electrically powered mixer with heat applied to the barrel was used to mix the sulfur and aggregate. Sulfur content of several mixtures was varied to obtain the best workability with a minimum of sulfur in excess of that necessary to fill the voids. The average grain sizes and grain-size distributions were also varied to determine their effects on strength. Unconfined compression tests of forty-five 6-by l2-inch cylinders yielded average strendths of 3,348 psi to 10,398 psi. The highest strength single cylinder was 10,717 psi. The cylinders were tested from 24 hours to 6 days after pouring; after 24 hours the rise in strength was very slight. From the results obtained it appears that sulfur can be a useful construction material. An evaluation was made of a high-vacuum application for sulfur concrete. Sulfur has a high vapor pressure at elevated temperatures, 50° to 100° C; consequently, significant losses by sublimation can be expected. At lower temperatures the losses are not significant; however, this factor will limit its use at a higher temperature.

Jan 1, 1970

By Karl C. Dean

All components of 15 automobiles manufactured between 1954 and 1965 were analyzed, and it was determined that a representative junk automobile would have the following composition (all figures in pounds): steel, 2,532; cast iron, 511; copper, 32; zinc, 54; aluminum, 51; lead, 20; rubber, 145; glass, 87; miscellaneous, 142. Time and motion studies and a cost evaluation were made to determine if such a typical vehicle could be economically burned in a smokeless incinerator and hand-dismantled, and if the resultant steel could be baled into a high-quality No. 2 bundle containing less than 0.10 percent copper. The cost evaluation showed that processing the composite car would cost about $51 to produce about $56 worth of marketable ferrous and nonferrous metal products and provide an annual rate of return on investment of 19 percent.

Jan 1, 1969

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 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 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 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 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 Robert E. Wood

The temperature dependency of the low-density viscosity coefficients, ?°T, of helium and of nitrogen, 100° to 1,000° K, is correlated with empirical equations, and the temperature and composition dependencies of the low-density viscosity coefficients, ?°T, of helium-nitrogen mixtures are correlated with the Chapman-Enskog expressions by using the Lennard-Jones (6:12) potential function. The residual viscosity, ?T,P - ?°T (the difference between the viscosity of a compressed gas and the dilute gas at a given temperature), was found to be a function of the thermal pressure coefficient, (?P/?T)V, and two parameters, a and 1, which are characteristic of gas composition. The equation ?T, P = ?°T + a [(?P/?T)V]ß represented 1,340 higher pressure experimental viscosity values with a mean absolute deviation of 0.86 percent, and this equation was used to compute viscosities of the gaseous helium-nitrogen system for a range of temperatures and pressures including those encountered in Bureau of Mines helium purification processes and in a crude-helium conservation gas reservoir. Tabular viscosities for helium, nitrogen, and 13 helium-nitrogen mixtures are presented for 110 temperatures, 133° to 740' K, and 49 pressures in the range 1 to 240 atmospheres. The accuracy of the tabulated viscosities varies because correlation parameters were obtained from experimental data of unequal reliability. It is estimated that uncertainties in the computed viscosity values are ±5 percent for the region 325° to 740° K, ±2 percent for the region 183° to 325° K, and ±5 percent for temperatures below 183° K. The latter uncertainty may rise to y10 percent as critical conditions are approached.

Jan 1, 1970

By K. Thirumalai

This study forms a part of Bureau of Mines continuing research on thermal fragmentation of rocks. The potential of internal heating techniques for rock fragmentation is discussed. A concept of rock fragmentation with rapid inter¬nal heating of a localized inner volume of rock is advanced The energy required for rock fragmentation is made available by creating a required vol¬ume of localized heating. The fragmentation of rock using the proposed method is analyzed and qualitatively compared with the results of experiments with Charcoal granite, Dresser basalt, and Sioux Quartzite. High frequency dielec¬tric heating below 100 MHz is used in the study as an example to examine the working of the concept. The selection of operating conditions for the experi¬mental heating is explained. Fragmentation of Charcoal granite and Dresser basalt test rock blocks is achieved for localized heating below 550° C. The heated volume required for fragmentation is observed to be less than 2 percent of the test block volume and the electrical energy consumption is in the order of 3.5 to 6 5 kwhr/m3 The method offers a possibility for in situ fragmenta¬tion of rocks, favorable for internal heating. The method is highly dependent on rock properties governing internal heat generation The efficiency of dielectric heating in the experimental study is observed to increase with increasing dielectric loss of the rock material, ranging from about 10 percent in Sioux. Quartzite to about 50 percent in Dresses basalt

Jan 1, 1970

By W. S. Sanner

Pyrolysis (destructive distillation) techniques developed at the Bureau of Mines to determine the yield and quality of the products from coal were used to convert municipal (household) and industrial refuse into potentially useful solids, liquids, and gases without adding to environmental pollution. The tests demonstrated that a ton of municipal refuse can be converted into 154 to 424 pounds of solid residue, 0.5 to 6 gallons of tar, 1 to 4 gallons of light oil, 97 to 133 gallons of liquor, 16 to 32 pounds of ammonium sulfate, and 7,380 to 18,058 cubic feet of gas. A ton of industrial refuse, consisting of paper, rags, and cardboard, can be converted to 618 to 838 pounds of residue, 1.5 to 3 gallons of light oil, 68 to 75 gallons of liquor, 12 to 23 pounds of ammonium sulfate, and 9,270 to 14,065 cubic feet of gas. The energy from the gas is more than sufficient to provide the heat for the pyrolysis.

Jan 1, 1970

By Donald R. Johnson

Apparatus providing simultaneous differential thermal analysis, thermo-gravimetry, and evolved gas analysis, has been developed by the Bureau of Mines specifically for thermal study of oil shale and other solid, natural fuels. The apparatus is described in detail, and simultaneous analyses on a single sample of an oil shale mineral, nahcolite, and a thermal analysis demonstration compound, calcium oxalate monohydrate, are presented to demonstrate the instrument's capabilities.

Jan 1, 1970

By Fred Leighton

The Bureau of Mines has developed rock noise source location techniques that may be used to obtain precise and practical source locations from micro-seismic field data. These techniques enable one to monitor all or any part of a rock structure and map progressive stress buildup or rock movement. Thus, the microseismic method of determining instability in rock structures is becoming an invaluable engineering tool for the mining or civil engineer engaged in rock excavation and construction.

Jan 1, 1970