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By Ralph B. Adair

The Bureau of Mines conducted laboratory and continuous pilot plant flotation tests to determine the feasibility of recovering commercial-grade mica from an Alabama graphitic-mica schist. Preconcentration of the ground ore on a Humphrey's spiral was employed to reject the heavy minerals and part of the quartz in a product virtually free of mica. The acid-cationic mica flotation process recovered over 89 percent of the mica in a product containing 98.7 percent mica. Grinding of the mica concentrate in a fluid energy mill produced a product with a bulk density of 12 lb per cubic foot.

Jan 1, 1969

By Mary A. Barrett

The Bureau of Mines conducted a laboratory-scale investigation of grouting mixtures containing iron or aluminum to determine the existence of health or explosion hazards, due respectively to oxygen depletion or hydrogen emission. Mixtures containing iron created an oxygen deficiency in less than 24 hours and released small amounts of hydrogen; a health hazard could occur but only under extremely unfavorable conditions. Mixtures containing aluminum released little hydrogen and consumed little oxygen; however, if improper on-site mixing yielded high local metallic aluminum concentrations, enough hydrogen might be released to produce an explosive atmosphere in a confined space.

Jan 1, 1969

By R. K. Koch

The vapor pressures of liquid titanium and liquid platinum were studied under the Bureau of Mines program for the determination of thermochemical data on the transition elements. Beating was done in a 2-kw electron-beam furnace with a water-cooled copper crucible to contain the melt. Temperature was measured with a disappearing-filament brightness pyrometer. The vapor pressure data for liquid titanium in the range 2,008° to 2,379° K are represented by the least-squares derived equation [log p (atm) = 6.268 - 22, T] Two series of determinations were made on liquid platinum. Results of the first series are expressed by the least-squares derived equation [log p (atm) = 8.240 - 30,460T] for the range 2,0860 to 2,4200 K. Results of the second series are expressed by the least-squares derived equation [log p (atm) = 7.795 - 29,580 T] in the range 2,045° to 2,442° K. Third-law evaluations of each series gave mean standard heats of sublimation of 112.4 kcal/mole, 133.3 kcal/mole, and 133.8 kcal/mole for titanium first series on platinum, and second series on platinum, respectively. Second-law heats of sublimation and equations for heats, free energies, and entropies of vaporization were obtained from sigma plots of each data set.

Jan 1, 1969

By M. O. Serbousek

To further investigate the potential of precast concrete sets as a support medium for underground mines, the Bureau of Mines designed an eight-piece precast reinforced concrete drift set for a small opening. Twenty-two sets of three different member sizes were tested to destruction under two loading conditions. A discussion of the test results and typical failure patterns is presented.

Jan 1, 1969

By R. S. Fowkes

The Bureau of Mines constructed a fully automated pilot plant facility to study the hydraulic transportation of solids through a lock hopper feeder system. An equation for the energy requirements to transport coarse solids hydraulically proved applicable to this system. Optimum velocities were obtained for limestone, mine refuse, and bituminous coal. The experimental data, calculations, and graphs show the effect of velocity, specific gravity, and solids concentration on head loss and power requirements. Other data were obtained and evaluated to determine the effect of particle size on head loss. Results also are given for (a) tests using friction reducing polymers; (b) tests using seven test sections of steel alloy pipe to determine their wear characteristics; (c) tests to determine spatial segregation of moving particles; and (d) tests to determine the effect of shape, size, and specific gravity on particle velocity in a horizontal pipeline. The lock hopper feeder system was found practical for continuous hydraulic transportation of the material types and size ranges tested.

Jan 1, 1969

By John Ward Smith

An analytical method developed by the Bureau of Mines to determine dawsonite, nahcolite, and nondawsonite alumina (called excess alumina) extractable from Green River Formation oil shales is presented. The method requires water extraction of nahcolite followed by HCI-extraction of dawsonite and an unidentified mineral yielding excess alumina from the water-leached residue. Instrumental determination of sodium in the water extract and sodium and aluminum in the HCI extract measures the sample's content of the minerals. Detailed evaluation shows the method to be adequately specific, precise, and reproducible and free from uncorrectable interferences. The method's results define precisely the production of sodium carbonates and alumina possible from a sample of oil shale and the interval it represents. Shale-oil yields, nahcolite contents, and yields of extractable alumina determined on 83 samples representing an 821-foot section of dawsonite-nahcolite-bearing shale from .Colorado Corehole No.3, drilled in the north part of Colorado's Piceance Creek Basin, are presented. These samples resulted in nahcolite contents to 53.3 percent, oil yields to 48.3 gallons per ton, and alumina yields to 5.80 percent. Use of these data to evaluate the production potential of a section of the formation are suggested.

Jan 1, 1969

By Danton L. Paulson

Elevated temperature electrical resistivity measurements were made by the Bureau of Mines on arc-melted, spin-cast, and hot-pressed columbium carbide¬carbon (CbC-C) and zirconium carbide-carbon (ZrC-C) materials up to 2,000° C. The CbC-C materials displayed electrical resistivity values ranging from 35.20 microhm cm at 23° C for hot-pressed material containing 12 wt pct carbon to 242.64 microhm cm at 1,622° C for arc-cast material containing 17.0 wt pct carbon. Electrical resistivity values ranged from 29 microhm cm at 20° C for arc-cast ZrC-C containing 16 wt pct carbon to 279 microhm cm at 1,951° C for hot-pressed ZrC-C containing 21 wt pct carbon. Data from a previous report were included to establish comparison between the electrical resistivities of the CbC-C, ZrC-C, and HfC-C systems.

Jan 1, 1969

By M. M. Fine

Research on the solid-fuel reduction of Knob Lake iron or was conducted to upgrade lean and high-grade ores and recover metallized products suitable for ironmaking or steelmaking. The program included bench-scale tests plus a number of continuous campaigns in a 34-inch by 36-foot rotary kiln. In the laboratory, metallizations in excess of 90 percent were achieved by reduction of crushed ore with lignite at 950° C. Subsequent grinding (to minus 200 mesh) and wet magnetic separation yielded concentrates analyzing less than 3.0 percent SiO2 and more than 90 percent Fe. Virtually complete recovery of the iron occurred. During early continuous tests the crushed ore created a serious ringing in the kiln which was solved by balling the fines with bentonite. Unfortunately, at this temperature (950° C) the bentonite militates against the concentratability of the metallized product. For example, a run on direct-shipping ore produced concentrates of 89.5 percent Fe and 4.5 percent SiO2. At 500° C the adverse effect of bentonite disappeared and concentrates of 88.4 Fe and only 2.5 percent SiO2 resulted. However, with comparable feed r Los, the metallization dropped to 73 percent.

Jan 1, 1969

By Foster Fraas

This Bureau of Mines report describes a method for separating minerals at magnetic susceptibilities within the diamagnetic susceptibility range. The maximum feed rate varies directly with the square root of the lower limit of permissible susceptibility, while the lower limit of permissible susceptibility varies inversely as the square of the magnetic field strength. Minerals may be separated at particle sizes smaller than possible on conventional dry-type magnetic separators.

Jan 1, 1969

By Clarence O. Babcock

Model pillars of limestone, marble, sandstone, and granite with length-to-diameter (L/D) ratios of 3, 2, 1, 0.5, and 0.25 (0.286 for granite) were tested to failure in axial compression to determine to what extent an increase in end constraint increased compressive strength. Adjustable steel rings, mechanically tightened about the ends of test specimens to create a radial prestress of 3,000 or 5,000 psi prior to the application of axial load, increased end constraint more than was possible in previous tests using solid steel rings. (Solid rings, epoxy-bonded to the ends of dogbone specimens, increased compressive strength compared with that of straight specimens without ring constraint.) During the loading cycle, additional end constraint was produced by lateral expansion of the specimens against the rings. The effect of the end constraint was to increase the compressive strength 55 to 58 percent for the shorter pillars of dogbone shape compared with the compressive strength of straight pillars with the same L/D ratios without ring constraint. Most pillars with L/D ratios of less than 2 were made stronger by end constraint. Pillars with an L/D ratio of 3 did not benefit significantly from end constraint. When the results from compression testing of straight specimens of rock in the laboratory are used to design mine pillars in situ, the pillars will be larger than necessary if the horizontal compressive stress is several thousand pounds per square inch greater than that resulting from the weight of the overlying rock alone. The L/D ratio can be increased by a factor of 1.76 for ratios in the range 0.25 to 3 and still provide the same compressive strength. The safety factor applied with straight specimen test results should also be acceptable for use with constrained pillar test results.

Jan 1, 1969

By L. C. George

The Bureau of Mines measured the vapor pressures of selected mixtures in the binary systems CdCl2 ?SnCl2, CdCl2 -ZnC12, PbCl2 ?SnCl2, and PbCl2 -ZnCl2 by the static pressure method. These data were evaluated by the second-law (sigma-plot) method. Equations expressing the vapor pressures and the heats and free energies of vaporization as functions of temperature are given.

Jan 1, 1969

By B. J. Dalton

The Bureau of Mines Helium Research Center has as a long-range objective the development of an equation of state for helium that will allow all of the thermodynamic properties to be calculated within the accuracy with which they are known. If this objective is to be realized, a method of calculation must be known. This report gives the principles of the method we use in such problems. A computer program was developed for predicting these properties, including those at the critical point, that is perfectly general and applicable to any equation of state. To demonstrate the efficacy of our method, this computer program was used to evaluate thermodynamic properties of a Redlich-Kwong fluid in the two-phase region. Expressions for calculating various thermodynamic functions specific for this particular equation of state are derived. Numerical values are tabulated and graphs are presented for all functions calculated. It is shown that for a Redlich-Kwong fluid there are finite discontinuities in (1) the second temperature derivative of the Gibbs free energy or chemical potential at the critical point, (2) the second derivative of the vapor pressure curve with regard to the temperature on passing through the critical point, and (3) the measured heat capacity at constant volume on passing through the critical temperature when the calorimeter is filled to the critical density. It is also shown that the heat of vaporization is infinite for a Redlich-Kwong fluid at absolute zero.

Jan 1, 1969

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

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove, grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 2 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

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 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 E. G. King

Low-temperature heat capacity determinations of the minerals goethite and pyrophyllite were made in the temperature range from 510 to 298° K. The entropies at 298.15° K were evaluated as 14.43 ±0.15 cal/deg mole for goethite and 56.6 ±0.5 cal/deg mole for pyrophyllite. The entropies of formation from the constituent oxides are -4.4 ±0.2 cal/deg mole for goethite and -12.3 ±0.6 cal/deg mole for pyrophyllite. The standard free energy of formation of goethite from its oxides is ?G°298.15 = 0.16 ±0.20 kcal/mole.

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 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