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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 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 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

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 Harold E. Marr

The Bureau of Mines evaluated two drill-hole probes for the delineation of Missouri lead ores. The battery-powered, portable instruments, weighing less than 30 pounds, were designed for logging holes of 1.8 inches in diameter or larger. These probes have dual scintillation detectors, balanced filters with a pass band for lead Ka radiation, and a cobalt-57 source of radiation. The results of field tests in Missouri confirm laboratory tests indicating that probe response can be correlated to lead ore grade using counting times of 10 seconds or less at any selected depth in the hole.

Jan 1, 1972

By R. B. Schluter

Drying and preheating (partial induration) the green, unfired iron ore pellets is a means of reducing the energy required to produce metallized pellets. The Bureau of Mines processed three magnetite and two hematite concentrates through the unit operations of pelletizing, preheating in air, and reduction to metal to determine the effects of preheating upon the properties of the metallized pellets. The pellets were prepared in a 16-inch-diameter laboratory balling drum. Preheating and metallization were carried out in an externally heated 4-inch-ID by 4-inch-long stainless steel drum using air for the preheating atmosphere and lignite char as a reductant. The results 'varied considerably: two of the magnetites spalled when preheated in air at temperatures of 900° C and above, and the third magnetite and the hematite flotation concentrate required complete induration at 1,300° C to produce satisfactory pellets. The earthy hematite ore yielded excellent pellets at all preheat temperatures.

Jan 1, 1972

By R. E. Peterson

Scrap iron is partially oxidized at elevated temperatures in the selective oxidation process to produce iron oxide and a dense residual metal of high purity. Investigation of the process was confined to converting automobile hulks into useful products. In one test series, compressed, sheared automobile scrap was processed at 1,000° C in a 36-foot-long rotary kiln at feed rates ranging from 300 to 1,200 lb/hr. Less fuel was required to maintain the temperature at the higher feed rates because of the heat generated from the burning of the combustibles and the oxidation of the iron. The bulk density of the residual metal exceeded 75 pounds per cubic foot. In an attempt to lower the quantity of contaminants in the residual metal, another test was designed using automobile hulks which had been prepared by ripping, a low-cost method of scrap fragmentation. Before oxidizing the ripped scrap approximately 62 percent of the total copper was removed in a tumbling, screening, magnetic separation and hand-sorting system. Cast iron made from the residual metal obtained by selective oxidation contained 0.15 percent copper; iron oxide scale obtained from the kiln averaged 0.13 percent copper. Pellets made from the scale demonstrated compressive strengths necessary for blast furnace reduction; lead and zinc were removed by volatilization when the induration was performed in a reducing atmosphere.

Jan 1, 1972

By Hillary W. St. Clair

This report gives the results of an experimental study of the progressive changes that occur in particle size and size distribution when a homogeneous and isotropic mineral is subjected to crushing by impact. The mineral used in the study was uniformly sized quartz, which was crushed in a simple drop¬-weight machine that applied impact energy up to about 100 kg-cm per g. Screen analyses of the crushed products were analyzed by the method of moments to determine the mean size, variance, skewness, and kurtosis. Analysis of the data from these experiments shows that the mean size of the crushed product is a function of the energy input and the initial size. The size distribution is functionally related to the degree of size reduction. As the mean particle size is decreased, at first there is a corresponding increase in the variance and decrease in the skewness, But, as size reduction is carried further, each tends eventually to approach a steady value, and the form of the size distribution becomes stable.

Jan 1, 1972