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By P. T. Brooks

This Bureau of Mines study describes a process for recovering nickel, cobalt, molybdenum, and chromium contained in complex waste superalloy grindings that, for lack of an economical domestic recovery process, are being largely marketed abroad. The process, devised by laboratory scale operations, includes scrap preparation, dissolution of metallics in hot chlorinated acidic liquor, carbon adsorption, three successive solvent extraction separations, and selective chemical precipitations. Nearly 90 percent of the nickel, cobalt, molybdenum, and chromium were separated and recovered as oxides, carbonates, and basic sulfate products.

Jan 1, 1969

By Jack L. Henry

The ternary system A14C3-AIN-Al203 has been examined to determine compositions which may display desirable high-temperature refractory properties. Powder methods were employed in the synthesis of all test compositions. Forming and sintering behavior was examined and hot-pressing parameters were measured. Several properties were studied for each composition of interest in the system. The properties included hydrolysis rate in moist air, elevated temperature oxidation rate, density, softening point, tensile strength, and rupture strength. In most cases equilibrium was not achieved, and the data are representative of a nonequilibrium system. Approximately 16 separate phases have been observed in the system. Forming behavior and selected properties of five compositions of interest were compared with those of aluminum oxide and aluminum nitride. None of the compositions compared favorably. Oxidation and vaporization appear to be serious drawbacks to the use of these compositions at elevated temperatures.

Jan 1, 1969

By R. S. Warfield

Several reconnaissance-type surface and drill core samples of Arctic Northwestern Alaska coals were taken during the summer field seasons of 1964 and 1966 for coking studies. Surface samples were taken from the Kokolik River and the Cape Beaufort areas; core samples were obtained from the Kukpowruk River and the Cape Beaufort areas. Only one Kokolik River surface sample possessed coking properties. This sample, representing an 11.6-ft coal seam, made coke approaching metallurgical quality when a 30-pct portion of selected blending coals was added. Four Kukpowruk River core samples, each representing the same 19-to 20-ft coal seam, were all of about the same coking quality. No differences of coke quality attributable to depth of permanently frozen overburden were found, but the data confirm previously reported information that the 19- to 20-ft coal bed is a potentially satisfactory base coking coal. In the Cape Beaufort area, a core sample with appreciable coking properties was taken at depth from a coalbed determined noncoking in a surface sample.

Jan 1, 1969

By Donald R. Corson

The effects of adding varying amounts of type I portland cement to hydraulic backfill are described. Six different fill materials, each with three cement contents, were tested to determine which fill properties have the most significant effect on cemented strength. Two strength prediction equations, based on the physical and mineralogical properties of the fills, were formulated, and these accounted for 96 and 99 percent of the variability of the data. Results of both unconfined compression and triaxial tests of cemented fills are given, and the effects of moist curing and fill densification on the 7-day strength are discussed. Permeability test data are given, and the decreased permeability due to cement content and curing time is shown graphically. A discussion of the limited evaluation of other potential stabilization additives (expansive cement, fly ash, sodium silicate, gypsum, and asphalt) is included in an appendix.

Jan 1, 1970

By F. S. Karn

Conditions necessary to obtain optimum yield of useful products when coal is rapidly heated to extreme temperatures by laser irradiation were determined by the Bureau of Mines. Product distribution and yield were investigated as functions of several variables. Low-rank coals with high-volatile matter gave highest total gas yields. Medium-rank coals gave the highest yields of H2 and CA and low-rank coals gave highest yields of CO and C02. Macerals gave gases of approximately the same composition, but the total gas yield increased in the order fusinite, micrinite, vitrinite, and exinite. Total gas and C2H2 yields varied inversely with particle size. The addition of nominally inert gases such as Ar, He, N2 increased yields of H2, C2H2, and total gas. Metals such as nickel and platinum had little influence on the rate of coal decomposition. Total gas yield increased with total energy of irradiation, and the ratio of C2H2-CH4 increased with concentration of energy. A study was also made of the irradiation temperature, and a material balance was calculated.

Jan 1, 1970

By Robert G. Lundquist

The Bureau of Mines compared longitudinal strain energy output of a percussive drill to energy determined by measuring maximum piston velocity. Strain gages were used to determine the strain-time waveform and its amplitude at seven levels of operating pressure and eight levels of thrust. The longitudinal strain energy was found to be approximately 14 ft lb less than the maximum piston energy at comparable operating conditions.

Jan 1, 1969

By Richard F. Hewlett

This report describes a comparison of methods for computing grade and tonnage of ore, leach, and waste material for a mined-out portion of the Silver Bell Oxide porphyry copper deposit, and these computed values are compared with the actual tonnage of these classes of material produced during mining operations. Comparisons with production records have been made by using both exploration drill-hole assays and development blast-hole assays. The polygonal method is the most accurate for this deposit, because it more closely represents the lateral mineral distribution in the deposit. This is demonstrated by plots of the total-copper assay distributions of the development blast-hole assays for a specific bench. The investigation also shows that the smaller vertical assay interval (based on a 5-foot vertical churn-drill-hole sample) yields a more accurate estimate of both grade and tonnage than the 40-foot composite assay interval (based on the average of eight 5-foot assay values). This can be attributed to the fact that selective mining within a bench can separate out much of the waste and leach material that is included as ore in the 40-foot composite assay computations.

Jan 1, 1970

By M. M. Fine

Chalcocite flotation concentrates (26-34 percent Cu and 6-7 percent S) were roasted in air to determine sulfur elimination as a function of temperature, airflow rate, and residence time. Fluosolids roasting was evaluated batchwise and continuously in a 4-inch fluid-bed reactor. Kiln roasting tests were carried out in a 4-inch ID by 6-inch-long rotary drum. Pelletizing the very fine concentrates prior to roasting was essential to minimize dust losses and accretions. Concentrate pellets, sized minus 10 plus 20 mesh and bonded with 2 percent bentonite, were excellent feed for fluosol¬ids roasting and limited dust losses to 10 percent or less. One-fourth-inch pellets were best suited to kiln roasting. Both techniques were capable of producing copper calcines analyzing well under 1 percent residual sulfur when operated at 900° C with average retention times of 3 to 4 hours. Calcined pellets were strong, porous, and readily reducible.

Jan 1, 1970

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 Robert L. Crosby

The Bureau of Mines investigated the substitution of cement copper powder for commercial copper powder in an Fe-7 pct Cu-l pct C powder metallurgy alloy. Copper powders from six different commercial cementation operations were separately upgraded by screening and hydrogen reduction. They were then mixed with commercial iron and graphite powders to form the Fe-7 pct Cu-l pct C alloy. Various chemical and physical properties were determined on the upgraded cement copper and the alloy powders. Mechanical, physical, and chemical properties were determined on green and sintered specimens made from the alloy powders. Mean tensile and bending strength of sintered specimens were significantly lower than the means from specimens made from commercial metal powders. The lower strengths are apparently related to poor sinterability.

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 J. E. Dooley

Reference mass spectra and analytical correlations for 20 alkylcycloalkyl sulfides and two dicycloalkyl sulfides are presented 'to provide information that will facilitate the identification of sulfur compounds occurring in natural or synthetic mixtures. Reference spectra indicate relative intensities in addition to parent and base peak sensitivities. Analytical correlations establish the ionic species that reflect major fragmentation paths for the com-pounds studied. Specifically, the correlations show that base peaks are formed by several different processes: (1) Cleavage of the bond a to the ring, (2) fragmentation of the alkyl chain, and (3) fragmentation of the ring plus fragment contribution from the alkyl chain. Useful correlations for deter-mining alkyl chain length involve the CnH2+3S+ and CnH2n+1 + ions. CnH2n-2+ and CnH2n-1 S+ ions reveal the number of carbon atoms in the cyclic ring. Other important ionic species are also discussed.

Jan 1, 1970

By Ted C. Briggs

Twenty-two compressibility runs were made with helium over the temperature range -5° to 80° C and at pressures to 800 atmospheres. A Burnett apparatus was used. Data from the runs were fitted to a fourth degree polynomial equation of state in the pressure and a weighting factor of Pr-3/4 was used. All data for a particular isotherm were treated simultaneously. A temperature function was found to represent the parameters B and C. Compressibility factors determined by this investigation are believed to be accurate to better than 0.05 percent.

Jan 1, 1970

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