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By L. B. Pankratz

Low-temperature heat capacities, high-temperature enthalpy increments, and the enthalpy of formation at 298° K were determined calorimetrically for vanadium subnitride (VN0.465). The low-temperature investigation gave S°298.15 = 6.379 ±0.005 cal/deg mole, and a combustion calorimeter investiga¬tion provided ?Hf°298.15 = -31.80 ±0.60 kcal/mole. The two quantities were combined with the high-temperature data to give standard values of enthalpies of formation and free energies of formation above 298° K. These and related thermodynamic functions were tabulated to 1,800° K. Similar data are included in the range of 298° to 1,600° K for the mononitride, VN.

Jan 1, 1971

By Larman J. Heath

Liquid incendiaries were burned within the interstices of several different types of sandstone cores to determine the technical feasibility of increasing sandstone permeability by this method. Fuel-oxidant mixtures were tested in 186 cores; six cores exploded when ignited. In virtually all instances, the explosion completely pulverized the sandstone cores. In addition n those cores damaged by explosions, 24 cores were fractured so severely that permeability tests were impossible. Although combustion gener¬ally increased the permeability, specific mixtures at given pressures were inconsistent in their ignition and burning behavior. Tests indicated that the heat of burning incendiaries significantly increased sandstone permeability. The improved permeability ratios were usually less than 2, but one was 10.3. Permeability alteration by other in situ methods was not as effective as that by flame propagation.

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 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 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 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 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

By N. N. Moebs

The atmosphere in part of an air-sealed coal mine was monitored continuously through a drill hole for oxygen content to determine the effectiveness of sealing a mine against the entrance of air and the major force that caused the phenomenon of mine breathing through the overburden. The differential pressure across the seal and the barometric pressure on the outside also were recorded. A general correlation, obtained between the oxygen level, differential pressure, and barometric pressure, indicates that changes in air pressure are the cause for periodic replenishment of the oxygen in the mine. Mine effluent quality was determined by conditions in many sections of the mine and could not be related to the oxygen level at the drill hole.

Jan 1, 1972

By G. L. Fitzpatrick

Preliminary results of an experiment in seismic holography indicate that the techniques of acoustical holography may be successfully used with seismic waves to determine the size and general shape of underground objects. This experiment was carried out under field conditions on a moderately large scale compared with the typical laboratory experiments in acoustical holography. The object to be mapped was a 100-foot-diameter, spherical, low-velocity zone of explosively fractured rock in oil shale at an average depth of 80 feet. The seismic wavelength of the Fourier component wave used in making the seismic holograms was 50 feet at a frequency of 140 cps. The hologram sampling aperture was 226 feet square and was sampled by 441 geophones in a 21 by 21 rectangular array. One novel aspect of the experiment was the use of a wide-band polychromatic explosive source of seismic waves rather than a narrow-band quasi-monochromatic vibrator source. A successful laser reconstruction of the object image from a lensless Fourier-transform hologram in the form of a 5/l6-inch-square photographic transparency is illustrated. The size of the underground object measured from the laser reconstruction of the object and the size inferred from a knowledge of the amount of explosives used to fracture the site and the tensile strength of the oil shale are found to agree.

Jan 1, 1972

By A. W. Deurbrouck

This report describes the washability characteristics of 18 coal samples taken from 11 drill hole cores from the San Juan Basin area of New Mexico and Colorado. The ash content of these coals could generally be substantially reduced by removing the heavy impurities. The coals were characteristically low in sulfur content; only one sample contained more than 1 percent sulfur after removing the sink-I.50 specific gravity material. The coals ranged in rank from subbituminous C to high volatile C; 11 of the samples were subbituminous A. Many of these core samples came from areas where very little fieldwork has been done; consequently, an outgrowth of this work has been an increase in known coal reserves of the San Juan Basin area.

Jan 1, 1972

By M. D. Schlesinger

Mercury exists in coal in minute quantities, but the large tonnages of coal consumed could represent relatively large amounts of mercury entering the environment. Limits have now been placed on the emission of mercury, and it is important that reliable analytical methods be available to the chemist. The Bureau of Mines has evaluated analytical techniques used by a number of laboratories; most used vapor phase atomic absorption as the final detection method. Neutron activation was used by some of the laboratories. All of the methods described could be applied, but they require careful manipulation to prevent loss or mercury contamination. In the samples analyzed the mercury content ranged between 0.05±0.01 and 0.4l±0.06 part per million.

Jan 1, 1972

By Foster Fraas

In this Bureau of Mines report, use of the photoemission of electrons to produce electric charges for the electrostatic separation of sonic dispersed minerals, which had previously been ground to pass a 43µ-opening sieve, is demonstrated. It appears that many of the oxides, carbonates, sulfides, and arsenides will respond to photoemission. Minerals least responsive are the oxides of silicon, the oxides of aluminum, and minerals that have a high concentration of these oxides. Although several synthetic ore mixtures did not yield to complete separation in a one-stage operation, it is probable that preliminary neutralization of the initial electric charges produced by powder dispersion will provide complete separation. That the separation can be carried out in air and without the use of reagents or heating, which are required in the present practice of electrostatically separating coarse granular feeds, is of special significance.

Jan 1, 1972