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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 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 J. D. Corrick

Research was conducted to develop operating techniques and define some of the limiting parameters for microbially converting hydrous calcium sulfate to hydrogen sulfide. The work was carried out in either glass stoppered flasks or anaerobic fermentors. Using the criteria of pH, temperature, number of bacteria per milliliter of test solution, and hydrogen sulfide produced, it was shown that hydrous calcium sulfate could be microbially converted to hydrogen sulfide at a rate of 7.3 g H2S/1 of fermentor volume per 24 hours. The various parameters defined were pH, temperature, and medium exchange rate. These were shown to be a pH range of 7.2 to 8.8, a temperature range of 30° to 35° C, and a medium exchange rate of 70 percent of the ferment or volume per 24 hours. It was also shown that a daily waste was between 50 and 77 percent as effective as sodium lactate in supporting the production of hydrogen sulfide and that by utilizing a gas to purge the fermentation system, a 1.7-fold increase in hydrogen sulfide was obtained.

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 T. E. Green

The Bureau of Mines Heavy Metals Program emphasizes the need for improved analytical methods for gold determination. A commercially available ion exchange resin with high selectivity for gold was investigated as a potential method to collect gold from solution. The resin was found to quantitatively collect gold from acid solutions over a wide range of acid concentrations. Common metals were not collected by the resin nor did they seriously interfere with the collection of gold. X-ray spectrographic and neutron activation methods based on the use of papers containing this resin are proposed.

Jan 1, 1970

By G. T. Brow

An experimental method is described for testing diffusion of gases in crude oils at pressures and temperatures up to 3,000 psia and 200° F. A sampling technique was developed to withdraw by constant-pressure mercury displacement about 60 µl of oil from the diffusion cell through any of several 1/2-in vertically spaced capillary tubes and to trap about 4 µl of the oil in a specially designed microsampler. Oil trapped in the microsampler can be completely inserted in the sample inlet of a chromatograph. From analysis in a three-stage chromatograph (GLC), gas concentration in a sample is determined from the ratio of gas peak heights to area of peaks of reference components (hexanes or heptanes) in the oil. A diffusion coefficient is calculated from measured concentration profiles with known equations for diffusion in finite or semi-infinite systems, depending on whether the gas has or has not reached the end of the oil column. Results are given for a test of methane diffusing at 2,560 psia and 160° F in crude oil from the Weber Sandstone reservoir in the Rangely field, Colorado. A constant diffusion coefficient of 3.34 X 10-5 cm2 per sec was obtained which gives a good fit between calculated and experimental profiles determined at six times after start of diffusion. The maximum standard error of gas concentration determinations experienced with this method was ±0.88 ml per ml of gas-free oil.

Jan 1, 1970

By F. P. Haver

A procedure is described for recovering both lead and sulfur from galena flotation concentrate, comprising the following steps: (1) Aqueous oxidation of the concentrate, using ferric sulfate to convert lead sulfide to sulfate and to give elemental sulfur; (2) regeneration of the ferric sulfate by electrolysis in a diaphragm cell; (3) treatment of the leach residue with ammonium carbonate solution to change the lead to an acid-soluble form and to produce ammonium sulfate as a byproduct; (4) solution of the lead carbonate in hydro-fluosilicic acid followed by electrolysis to recover the lead as metal and regenerate the acid; and (5) extraction of the elemental sulfur from the final residue with an organic solvent. About 90 percent of the lead can be recovered by the above method as 99.9-percent-pure metal, together with two-thirds of the sulfur--half in the elemental form and half as ammonium sulfate.

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 A. R. Rule

Laboratory tests were conducted to study removal of magnesium impurities from western phosphate rock concentrates by selective leaching. The systems evaluated included leaching with dilute sulfuric acid, with ammonium sulfate, and in an aqueous medium with sulfur dioxide gas. Set standards for the magnesium impurity level of phosphate rock concentrates are not available, but industrial practice has indicated that magnesium in excess of 0.3 percent MgO causes problems in phosphoric acid manufacture. Removal of magnesium was accomplished with all three systems. With dilute H2S04 the magnesium level was reduced to less than 0.1 percent MgO with an accompanying P205 loss of 6 percent. Magnesium oxide levels from 0.3 to 0.2 percent were obtainable with ammonium sulfate. However, the system requires concentrate roasting at temperatures of 900° C or higher, heated pulps (100° C), and large quantities of ammonium sulfate. Selective leaching was obtained using S02 gas in an aqueous concentrate slurry. Magnesium oxide content was reduced to less than 0.1 percent without loss of phosphate.

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 J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of three samples collected from the Kidney seam, in the Northern Field of the anthracite region. Removal of the sink 1.70 specific gravity material from the samples collected would result in greatly reduced ash contents at yields in excess of 90 percent. The Kidney seam, in the locations sampled, proved to be a low-ash anthracite containing an unusually high percentage of float 1.45 specific gravity material.

Jan 1, 1970

By Carl E. Norman

An investigation of geologic structure on macroscopic, mesoscopic, and microscopic scales was conducted on near-surface igneous and metamorphic rocks in which the existing stress field was determined by in situ methods. A consistent NE-SW orientation of the maximum compressive stress in the horizontal plane at four of five test localities appears due to the intrusion of NW-trending diabase dikes. Structural features at the mesoscopic scale show no consistent directional relationship to determined stress directions. Petrofabric diagrams of open microfractures show preferred orientations, but these are not consistently related to the orientations of larger structural features, such as joints, foliation, or mineralized shear zones. However, at five of six test sites the preferred direction of microfractures occurs nearly perpendicular to the maximum principal stress directions; an anomalous parallel relationship exists at a test site in an intrusive rock body. The results suggest that the open microfracture subfabric may provide a means for gaining information on the directional properties of stress fields. Such information can be obtained from oriented cores taken from holes which exceed the approximate 100-foot depth to which other in situ methods are presently limited.

Jan 1, 1970

By Ted C. Briggs

A removable-jacket distortion apparatus was constructed and used to measure distortion coefficients for two high-pressure vessels. The measured distortion coefficients were used to compute distortion coefficients for volumes VI and (V1+V2) of a 1,000-atmosphere Burnett compressibility apparatus for the temperature range 0° to 75° C. Young?s modulus for Armco 17-4 PH stainless steel, heat treated to condition H1150-M, was computed from experimentally determined distortion coefficients. A 10-to 14-percent correction to the values obtained for Young's modulus may be required because pressure vessel end effects were neglected. The distortion coefficients of the compressibility apparatus are believed to be accurate to about 1 percent.

Jan 1, 1970