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By J. W. Town

The Bureau of Mines determined the physical properties of southeastern Idaho phosphate fines as related to mineral composition, particle size and liberation, beneficiation, and potential use in structural clay products. The phosphate mineral in the fines was identified by unit-cell dimensions to be essentially the same as the phosphate mineral fluorapatite identified in the coarser sizes. The mean particle frequency as determined by electron-microscopy and pipet-analyses was between 0.5 and 0.2 micron. Liberation of the phosphate could not be definitely determined because of the weathered condition of the minerals and their extreme fineness. No beneficiation scheme was developed that would concentrate the phosphate into a marketable fertilizer product; therefore, forming and firing tests were made to demonstrate that the fines can be used to manufacture structural clay products.

Jan 1, 1968

By S. J. Aresco

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 instruction3 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, 1969

By John M. Gomes

The preparation of tungsten carbide by molten-salt electrolysis was investigated. Sodium tungstate in the electrolyte and carbon from the graphite anode were the source materials, Optimum results were obtained with an electrolyte consisting of 83 mole-percent sodium chloride and 5.7 mole-percent each of sodium tungstate, sodium metaborate, and sodium hydroxide; a temperature of 1,000° to 1,025° C; an anode current density of 37 amp/dm2 or less; and an initial cathode current density of 150 amp/dm2. The yield was approximately 0.45 g/amp hr. The electrolytic tungsten carbide product contained approximately 5.4 weight-percent combined carbon as compared to 6.1 weight-percent for pure tungsten carbide. Microhardness of the electrolytic tungsten carbide, determined with a 50-gram load, varied from 3,480 to 3,970 dph. The material was friable and could be ground in a laboratory ball mill to less than 400-mesh particle size.

Jan 1, 1969

By Merle L. Bowser

The Bureau of Mines has developed a portable recording methanometer that utilizes the Bureau's methane sensor. The methanometer can operate continuously for at least 30 hours on small, sealed, rechargeable lead-acid batteries.

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 K-H. Frohne

This report presents a study of the Cooper sand of the Fork Run pool of Warren and McKean Counties, Pa., and a prediction of the secondary oil recovery by gasflooding the reservoir. A computer program employing a modification of the Craig, Geffen, and Morse secondary recovery calculation was used to make the gas flood performance forecast and is presented in the appendix. The Cooper sand reservoir in the Fork Run pool lies at a depth of about 1,900 feet and covers an area 1/2 mile wide by 2-1/4 miles long. Original oil in place is estimated to have been 8,266,000 STB. The primary recovery mechanism is solution gas drive, and ultimate primary recovery may reach 20 percent over a well life of 90 years. Two computer predictions were made for gas flooding the Cooper reservoir. The first was for a 25-acre pilot five-spot utilizing existing wells, but project economics were poor since only 25 percent of injection gas is utilized for pilot oil recovery. Recovery was 71,000 STB, or 22 percent of oil in place at flood initiation, but required 25,700 scf gas injected per STB of oil recovered. In the second prediction, pilot area performance was projected for the entire Fork Run pool, and economics became good. Recovery was 1,753,000 STB from 25 five-spots after the injection of only 6,400 scf per STB of oil recovered.

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 J. S. Miller

The Bureau of Mines conducted surface tests to determine the feasibility of using liquid explosives for underground rock fracturing. The effects of configuration, confinement, length, critical layer thickness, and fracture-propping sand on detonation and explosive propagation velocity of desensitized nitroglycerin were studied, using polymethyl methacrylate and glass-plate reservoirs through lengths from 3 to 12 ft, with explosive-layer thicknesses from 0.1875 to 0.0312 in and in aluminum tubes 8 ft long with diameters from 2.000 to 0.125 in. Interval and continuous detonation velocity data were obtained. Under the test conditions detonation velocity was dependent upon explosive confinement and fracture-propping sand. The detonation velocity of a confined nitroglycerin explosion in aluminum tubes can be reduced by as much as 85 percent, when the tube contains fracture-propping sand. The shape of the reservoir, whether triangular or rectangular, has little effect on the detonation velocity or explosive propagation. The critical or minimum explosive-layer thickness between glass plates, capable of supporting propagation, was 0.0312 in. The presence of a fracture-propping sand in the sheetlike layers increased the critical explosive layer thickness to 0.0625 in. In nitroglycerin-filled and nitroglycerin-sand filled tubes, the minimum tube diameters successfully tested were 0.125 in and 0.375 in, respectively.

Jan 1, 1969

By M. M. Tilman

In a Bureau of Mines investigation to develop lead alloys with improved tensile strength and creep resistance, lead-base alloys containing cadmium and antimony in nominal 1-to-1 atomic ratios were melted in air, cast, and rolled into sheet to 90 percent reduction at temperatures varying from room temperature to 175° C. Tensile testing at room temperature and stress-rupture testing at 900±3° F were conducted on the as-rolled alloys. The best tensile properties were observed in an alloy of Pb-4.2 wt pct Cd-4.5 wt pct Sb which exhibited an average tensile strength of 7,270 psi with 36 percent elongation in 2 inches. An alloy of Pb-5.5 wt pct Cd-6.0 wt pct Sb had 100-hour stress-rupture values of approximately 2,100 psi and 1,000-hour values of approximately 1,700 psi.

Jan 1, 1969

By Richard Havens

Acidic and basic uranium leach plant residues located on the Navajo Indian Reservation, Tuba City, Ariz., were successfully stabilized against wind erosion using a relatively low-cost chemical method. An elastomeric polymer chemical was applied to the dike areas and a calcium magnesium lignosulfonate to the beach areas of three tailings ponds. The water-soluble chemicals were applied with an automated sprinkling system. The stabilization cost was $335 per acre for the 34.5-acre tract.

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 Donald C. Strimbeck

The Bureau of Mines designed a down-fired refractory-lined combustor that efficiently burned pulverized coal to produce a gas suitable as working fluid for an open-cycle gas turbine. The gas contained relatively little carbon, so the load on the ash-separation equipment was significantly reduced. Moreover, reduction in carbon content of the gas increased the average density of the solid particles making them more amenable to removal by centrifugation. Centrifugal-type separators failed to remove sufficient ash; however, to limit blade wear enough to achieve operating periods generally deemed necessary for commercial practicability.

Jan 1, 1969

By C. A. Komar

The Bureau of Mines conducted oil-displacement tests in the laboratory with three water-in-oil and five oil-in-water emulsions that were created with ultrasonic energy at a frequency of 20 kHz and an acoustic intensity of approximately 100 watts per cm2. Emulsions of either crude oil or kerosine, brine, and 112 to 2 percent emulsifier were formed during 30 seconds of acoustic irradiation. Results indicate that ultrasonic energy induces greater and more uniform dispersion of one liquid in another in the presence of small amounts of chemi¬cal emulsifiers. When the emulsions were injected as a buffer slug before waterflooding, recovery of the oil-in-place was 8 to 22 percent greater than with conventional waterflooding in the test specimens, regardless of the con¬tinuous phase (oil or brine). The emulsions do not appear to be applicable to the Appalachian area; however, because the oilfields are too "tight," the clays in the formation remove the emulsifier from the displacing fluid, and not enough additional oil is produced, compared with recovery using conventional waterflooding, to warrant the increased operating costs.

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 S. E. Khalafalla

The Bureau of Mines investigated the metallothermic reduction of copper oxide as a function of temperature, reactant proportions, form of reductant, and gaseous environment, using iron and steel scrap reductants. The reaction proceeded rapidly with powdered iron at temperatures above 560° C, attaining over 95 percent copper metallization within 3 hours. The importance of inter-reactant contacts on the extent of the reaction was evident from the variable, but usually lesser, degree of metallization obtained with iron from tin cans and automobile steel scrap. Reduction decreased as the molar ratio of copper to iron increased between 1 and 3. The most favorable gaseous environment for the reaction was a static helium atmosphere containing about 0.6 percent water vapor. Ferrothermic extraction of copper from its oxides appears to be essentially a "solid-state cementation" process. While ordinary cementation processes must be preceded by leaching, the ferrothermic method avoids this generally slow step and also the water pollution caused by the leaching agents. Sulfidic copper concentrates could likewise be reduced with metallic iron following their complete oxidative roasting.

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 H. D. Jacobs

The Bureau of Mines developed a concentration method to upgrade and utilize marginal natural or direct-shipping iron ores and fine-grained lean iron ores. Presently these ores receive little beneficiation and accordingly have low iron-silica (Fe-Si02) ratios. Ore samples were roasted with equal weights of solid reductant at 1,100° C for 1 hour to metallize the iron and for an additional hour at 1,200° C to promote grain growth. Concentration was effected by crushing and screening techniques and/or wet magnetic separation. Sized concentrates (minus 4 plus 35 mesh) derived from crushing-screening processes contained from 80 to 85 percent iron that was 90 percent metallized. Iron-silica ratios as high as 12:1 and iron recoveries from 75 to 94 percent were obtained. The sized concentrates were judged suitable for use as blast furnace feed. Minus 200-mesh metallized concentrates derived from roasted minus I-inch plus 8-mesh ore fractions and magnetically concentrated contained 90 percent Fe and 4 percent or less Si02, chemically qualifying them as feed for electric furnaces. Roasting minus 8-mesh ore with hydrogen, then magnetically concentrating it, produced iron concentrates containing 57 percent to 67 percent Fe and 3.6 percent to 8.4 percent Si02. The concentrates having Fe-Si02 ratios ranging from 8:1 to 12:1 were considered adequate for use as blast furnace feed. Overall iron recoveries for the 12 ores tested ranged from 56 percent to 94 percent with an average iron recovery of 86 percent.

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