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By D. G. Kesterke

Research was conducted to determine the feasibility of extracting elemental oxygen from silicate-bearing melts by high-temperature electrolysis. The method was based on a modification of existing processes for electrowinning metals from their oxides dissolved in molten halide systems. Electrolyses were performed at temperatures ranging from 1,050° to 1,250° C in boron nitride cells that incorporated a silicon carbide cathode and an iridium anode. The electrolytes contained volcanic scoria as the oxygen source, plus mixtures of BaF2 and LiF as fluxing agents. Cell gases containing almost 14 volume-percent oxygen were obtained. The average anode current efficiency for several experiments of extended duration was calculated to be 55 percent. Cell design and operating conditions are described, and some of the problems associated with the process are discussed.

Jan 1, 1971

The Bureau of Mines has long 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 instructions1 issued by the Bureau of Mines, and 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. The Government, with the exception of the Tennessee Valley Authority, purchased approximately 5.5 million tons of coal in fiscal year 1971. In connection with these purchases, the Bureau analyzed 4,366 samples. These are published (table 1) for the use of Government officials and the public. Such analyses of 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, 1972

By Verne E. Hooker

Near-surface temperature measurements in two granite quarries show that diurnal temperature variations are significant to a depth of 1 or 2 feet, and annual temperature variations are significant to a depth of at least 25 feet. As a result, ground stress anomalies due to temperature exist near the surface, and their magnitude depends upon the time of day and the time of year. Rock stress and corresponding temperature measurements were made in one granite quarry over a rock temperature range of 33° to 81° F. Measured rock temperatures show good agreement with values predicted from one-dimensional heat flow theory. Calculated and measured stress-temperature coefficients for the two granites in this study are given. Thermally induced stress variations in near-surface rocks tested were as large as 1,690 psi from combined daily and seasonal temperature changes.

Jan 1, 1971

By D. G. Kuehn

Positive ion sampling studies have been conducted on do discharges containing 0.33 percent sulfur dioxide in helium. Measurements were made for normalized gas pressures from 0.45 to 6.8 torr and discharge currents from 5 to 40 ma. Ion species observed included SO+, S+, SO2+, SO3+; O+, and 0+, 02+. Studies were conducted on the functional dependence of the various ion species with respect to axial distance, pressure, current, and gas flow rate. Interpretation of these results is consistent with the assumption of SO2 dissociation. Deposition of sulfur compounds was observed in the plasma container during these studies. The present results are compared with previous studies which have been conducted in SO2.

Jan 1, 1971

By Charles Findlay, Stephen Krickovic

A methane emission rate study was conducted in 1969 on a longwall section of a Lower Kittanning coalbed mine in central Pennsylvania. The longwall face was mined with a drum shearer between developed headings on the head end and headings on the tail end that were driven with a ripper-type continuous miner as needed. The study was conducted over 22 consecutive shifts (7-1/3 days). The average methane emission rate from the Lower Kittanning coalbed during mining at the face and developing the headings at the tail end of the face was 34 cfm. Caving of the gassy overlying strata as the result of mining at the face increased the methane emission to rates ranging from 702 to 1,049 cfm.

Jan 1, 1971

By Stephen Krickovic

A methane emission rate study was conducted in 1969 on a longwall section of a Lower Kittanning coalbed mine in central Pennsylvania. The longwall face was mined with a drum shearer between developed headings on the head end and headings on the tail end that were driven with a ripper-type continuous miner as needed. The study was conducted over 22 consecutive shifts (7-1/3 days). The average methane emission rate from the Lower Kittanning coalbed during mining at the face and developing the headings at the tail end of the face was 34 Am. Caving of the gassy overlying strata as the result of mining at the face increased the methane emission to rates ranging from 702 to 1,049 cfm.

Jan 1, 1971

By Thomas E. Green

A gas volumetric method was developed for determining metallic aluminum at the 0.01-to 0.3-percent level in 100-gram samples of recycled glass. The method is based on the measurement of the change in gas volume produced by the reaction 2 Al + 2 NaOH + 2 H2O ? 2 NaAl02 + 3 H2 using a simple apparatus assembled from readily available glassware. Apart from sampling errors, the precision of the method is within ±5 percent. A minor modification of the apparatus would extend the method to larger samples or samples of higher metallic aluminum content. Metallic iron and metallic zinc do not interfere at the concentrations found in recycled glass recovered from incinerator residues.

Jan 1, 1971

By J. M. Kuchta

Ignition and flammability test methods were developed by the Bureau of Mines for use in the classification of flammable solids by the Department of Transportation. A rotating disk ignition apparatus and a flame-spread-rate apparatus are proposed for determining the ignitability and flammability, respectively, of most flammable solids. Extremely flammable solids, such as pyrophoric materials, are evaluated by determining their ease of spontaneous ignition in an environmental chamber at high-humidity conditions. Data are presented for various representative solids to show the reliability of the test methods for classifying the materials. A classification system is also proposed for use in government transportation regulations.

Jan 1, 1972

By J. M. Kuchta

Bench-scale test methods were developed by the Bureau of Mines for use by the Department of Transportation in the classification of solid and liquid oxidizers. A burning rate test is recommended for evaluating the fire hazard of solid inorganic oxidizers when mixed with a red oak sawdust as the reference combustible. A spontaneous ignition test is proposed for evaluating liquid and solid inorganic oxidizers which may decompose violently or ignite spontaneously when unmixed or mixed with the wood sawdust under unconfined conditions. Test results are compared for various representative oxidizers and a classification system is proposed for use in the government transportation regulations.

Jan 1, 1972

By James H. Scott

A technique of seismic refraction data analysis has been developed in which a digital computer is used to generate a two-dimensional model representing a layered-earth depth interpretation. Travel times are picked on seismic records by the human interpreter. These times, together with shot point and geophone locations and refraction layer control information, are submitted to the computer on punched cards. A first approximation delineation of each refraction horizon is obtained by a computer adaptation of the delay-time method. The approximation is then tested and improved by the computer through the use of a ray-tracing procedure in which ray travel times computed for the model are compared against field-measured travel times. The model is subsequently adjusted in an iterative manner so as to minimize the discrepancy between computed and measured travel times. The Fortran program is listed in the appendix of the report together with instructions for preparing data cards and examples of results.

Jan 1, 1972

By H. E. Thomas

[The Bureau of Mines has conducted a field hydraulic fracturing experiment to determine the preferential orientation of induced fractures in oil shale at a depth of about 400 feet in the Green River Basin of Wyoming. The hydraulic fracturing treatment was performed by injecting extremely viscous water-base gel and 8- to 12-mesh sand into the oil shale through straddle packers set in an impermeable section of smooth-walled, 6-1/4-inch-diameter open hole. An impression packer proved that a horizontal fracture, which has an average width of about 1/2 inch at the borehole, was induced. A corehole drilled 100 feet from the fractured well intersected the fracture and confirmed its horizontal orientation. Because a horizontal fracture was successfully initi¬ated, it is inferred that the creation of multiple, closely spaced horizontal fractures may be feasible in Green River Basin oil shale.]

Jan 1, 1972

By B. J. Scheiner

Oxidation procedures based on the chlorine-hypochlorite system were investigated for improving gold recovery from carbonaceous gold ores. The oxidation pretreatment prior to cyanidation was accomplished by (1) addition of sodium hypochlorite to ore pulp, (2) by addition of chlorine to ore pulp, and (3) by generation of hypochlorite in situ by electrolysis of a brine solution used to pulp the ore. Gold extraction of 90 pct was achieved by cyanidation of carbonaceous ore that had been pretreated with 20 Ib per ton sodium hypochlorite at 50° C for 4 hours. Similarly, pretreatment of the ore pulp with 35 1b chlorine per ton at 24° to 30° C and 15 hours reaction time resulted in 89-pct gold extraction by subsequent cyanidation. Concomitant studies showed that electrolyzing the pulp prepared with a brine solution was equally as effective as electrolyzing hypochlorite and chlorine for oxidizing carbonaceous ore constituents that are deleterious to cyanidation. Gold extraction of 90 pct was obtained by electrolysis when 275 lb of are was treated at 200 amp for 7 hours in an 8-to 10-pct salt solution. Power consumption was in the range of 60 kwhr per ton.

Jan 1, 1972

By Harold L. Rhodes

Vapor-liquid equilibria data for 65-34-1 and 25-27-48 mole percent helium-nitrogen-methane mixtures are presented for 12 temperatures from 76.5° to 164° K and pressures from 100 to 1,200 psia. These data were obtained in a windowed phase equilibria cell equipped with a vapor recirculating pump. Isobaric and isothermal K-values are plotted for both mixtures. Two isometric plots are included.

Jan 1, 1972

By Charles C. Boley

High-volatile A bituminous coal from the Allen mine, Las Animas County, Colo., blended with char produced from the same coal yielded accept-able metallurgical coke in a 500-lb movable-wall test oven. Nineteen experimental runs were carried out using several concentration levels of two different chars, 5.6 and 19.6 percent volatile matter, produced by entrainment carbonization of the base coal. With the higher-volatile char, an acceptable coke was produced at a 22.5-percent concentration; the lower-volatile char did not produce an acceptable coke at the concentrations investigated.

Jan 1, 1972

By M. J. Ferrante

Enthalpy and entropy increments above 298.15° K were determined for cop-per sulfate between 298° and 1,000° K and for copper oxysulfate between 2980 and 1,146° K by the method of copper-block drop calorimetry. Enthalpies, entropies, and heat capacities are tabulated for both compounds. In addition, free-energy functions are tabulated for the sulfate. Equations representing the enthalpies are given for each compound.

Jan 1, 1972

By W. E. Lamont

Flotation studies of phosphate-bearing waste pond materials, low-grade washer products, and raw ores, all from the Tennessee brown phosphate district, showed that these types of materials could be treated without des liming to recover high-grade phosphate concentrates. The investigation showed that fine grinding before flotation was a requisite for increased recovery of the phosphate values and that the optimum pH conditions were in the range of 10.0 to 10.5 when using anionic collectors. Multiple-cleaning of the rougher phosphate concentrate was required to produce high-grade concentrates. Phosphate recoveries ranged from 60 to 82 percent and were inversely related to the grade of concentrate produced.

Jan 1, 1972

By D. Montagna

The Kroll-Betterton process for debismuthizing lead is based on adding calcium and magnesium to impure molten bullion to form solid Ca-Mg-Bi inter-metallic compounds that float on the surface as drosses. Present practice in industry is to hand-skim off these drosses, often followed by hydraulic pressing to squeeze out some of the entrapped liquid lead. In an effort to develop an improved technique, the use of an argon-shrouded dipping centrifuge to perform the required phase separation was investigated. Centrifugation experiments demonstrated that the bismuth content of an impure bullion could be lowered from an initial 0.5 percent down to 0.03 percent with a lead recovery of 90 percent, which is comparable to lead recovery after hand skimming of drosses in commercial lead-debismuthizing operations. Centrifugation provides better control in removing drosses, faster operation with less oxidation and relatively little fuming, and recovery of a lead bullion that approaches commercial specifications.

Jan 1, 1972

By E. L. Singleton

The Bureau of Mines investigated extraction of aluminum from aluminum-silicon alloys as a means of utilizing domestic aluminum silicate ores for aluminum production. Aluminum was extracted from aluminum-silicon alloys by electrolysis in molten electrolytes of NaCl-KCI-AIC13 and NaCl-KCI-AIF3 in a laboratory-scale cell. Six alloys with aluminum contents ranging from 20 to 87 percent aluminum were tested, and aluminum products of primary grade or better were obtained. More than 80 percent of the aluminum was recovered with current efficiencies as high as 91 percent. Recovery of a metallurgical-grade silicon product from the anode residue by an acid leaching procedure was possible with the 50-50 and 65-35 Al-Si alloys.

Jan 1, 1972

By J. E. Dooley

A mass spectral scheme of analysis was devised which can be used to identify individually a single compound from a larger group of similar compounds. Mass spectra for 32 alkyl aryl sulfides are provided for future reference work, and analytical correlations used in producing the analytical scheme are discussed. Some of the correlations show that base peaks are either the same mass as the parent peaks or may be derived from cleavage alpha to the sulfur atom with migration of one hydrogen to the sulfur atom. Other spectral consistencies provide means of separating ortho-, meta-, and paratolyl arrangements in an overall analytical scheme. Determinations of chain lengths and separation of isomeric species are also discussed.

Jan 1, 1972

By M. E. Tyrrell

The Bureau of Mines produced building brick of good quality in an investigation designed to explore the possible utilization of high-glass fractions of municipal incinerator residues in the manufacture of building products. Common clays, lime, and sodium silicate were used as binders for the nonplastic residues Test bricks were formed by dry-pressing, soft-mud molding, and stiff-mud extrusion. A run of standard-size face brick dry-pressed and fired in the West Virginia University Coal Research Bureau pilot plant demonstrated that SW-grade glass-clay face brick can be produced on a commercial scale without difficulty. A cost evaluation made for production of the brick showed an estimated cost of $42.13 per thousand bricks for a shuttle kiln plant and $28.70 per thousand for a tunnel kiln plant.

Jan 1, 1972