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By J. S. Miller

The Bureau of Mines developed methods for fragmenting oil shale formations with chemical explosives to prepare oil shale for in situ retorting and to evaluate the extent of fragmentation by various methods. A combination of three methods of explosive fracturing was used: (1) The displacement and detonation of a liquid chemical explosive in a natural fracture system; (2) the use of 60-pct dynamite to relieve stress conditions of the rock around the wellbore; and (3) the use of pelletized TNT in a series of wellbore shots to fragment the oil shale. An attempt was made to seal or grout around the fragmented oil shale by drilling 67 holes and displacing approximately 200 bbl of neat cement in the fracture system to aid in evaluating the fragmented zone, Seven methods were used to evaluate the fragmented zone. The primary evaluation method was the recording of seismic waves to delineate the fragmented zone with results based on arrival time, amplitude, and record quality. The data from the seismic measurements indicated the extensively fragmented zone was approximately 95 ft in diameter and 70 ft thick. Results of the remaining methods of evaluating fractures--including air-flow tests, coring of the expected fragmented zone, elevation measurements to indicate overburden crowning, and surveys with high-speed camera, impression packer, and down-hole camera--agreed with and supported the data from seismic measurements. Further field application of explosive fracturing and evaluation methods is needed to determine when a zone of oil shale is effectively fragmented for efficient in situ retorting.

Jan 1, 1973

By W. W. Agey

The Calico silver-barite deposits near Barstow, Calif., are a potentially important resource. Exploration performed by two major mining companies out-lined large tonnages of ore that assayed at 2 to 3 ounces of silver per ton and 7 to 15 percent barite. Laboratory beneficiation work was done by the Bureau of Mines on four samples to develop methods for recovering the silver and/or barite. Cyanidation recovered from 47 to 60 percent of the silver from ore ground to approximately 100 percent minus 325 mesh. Salt roasting minus 10-mesh material, followed by regrinding and cyanidation, recovered 75 to 85 percent of the silver. From 75 to 90 percent of the barite was recovered in a plus 92-percent barite product from either the natural ore or from cyanidation residues. Salt roasting before cyanidation precluded recovery of the high-grade barite concentrate from the leach tails.

Jan 1, 1973

By G. A. Wancheck

Shear tests were performed on several prepared samples of granular and powdery bulk materials to investigate the following parameters: Particle size and distribution, particle movement, moisture content, consolidation of material, bulk density, void ratio, porosity, volume change, and strain rate. A series of shear tests was performed with weight-percent-ratios of minus 0.185-inch tertiary sand and 1-1/2-by l/2-inch tertiary gravel mixtures, and weight-percent-ratios of minus 200-mesh limestone (rock dust) and minus 200-mesh bituminous float coal dust. A comparison was made for shear test results obtained with rectangular and circular shear cells utilizing the large and small direct shear testers. Specifically, the shear results obtained include the angle of internal friction or shear strength of the tested material under known consolidating pressures, and the kinematic angle of friction or coefficient of friction between the interface of a bulk material and a sample wall material. The experimental procedure, tests, and results are given for each parameter investigated.

Jan 1, 1973

By W. T. Abel

The difficulties associated with wet-processing fine size coal led the Bureau of Mines to investigate a dry process for removing pyrite from coal pulverized to powerplant fineness. The dry process that was investigated consists of two cleaning steps: First, centrifugal separation is used to remove a fine, pyrite-depleted portion as a product; second, the remaining coarser, pyrite-enriched portion is taken to electrostatic separation in which pyrite is concentrated and rejected. Ball milling and Hardgrove milling were used to pulverize the coal. Three coals from the Pittsburgh seam were treated by the dry-removal process. Over 55 pct of the pyrite, which amounted to 70 pct of the available pyrite, was removed in a reject of 10 to 20 pct from one of the coals. Similar treatment of the other two coals removed about 35 to 50 pct of the pyritic sulfur, which amounted to about 70 pct of the available pyritie, sulfur from these coals. Both centrifugal and electrostatic separations were more efficient when pyrite particles were as large as possible. Separation efficiency was improved by confining the particle size of the feed to a relatively narrow range and by avoiding excessive amounts (more than 10 pct) of dust in the electrostatic range. The removal efficiency was increased with the use of stage grinding.

Jan 1, 1973

By J. R. Ross

The extraction and recovery of nitrate from waste solutions generated in the production of titanium were investigated using solvent extraction techniques. Laboratory studies and continuous tests in a small solvent-extraction system showed that up to 98 percent of the nitrate can be selectively extracted by a solution of tributyl phosphate in kerosine. The extracted nitrate can be recovered as nitric acid, at concentrations suitable for reuse, by stripping the loaded organic with water.

Jan 1, 1973

By J. R. McVey

A 10-channel automatic data acquisition system has been designed and environmentally packaged for use with underground strain-gage applications and associated instruments. The system uses commercially available components and is assembled in two plastic enclosures. Environmental control is provided through a specially designed (compressed-air) air-conditioning system and water-resistant cabling. Accuracies of 0.01 pct and resolution of 1 µV have been obtained in underground tests.

Jan 1, 1973

By F. W. Penn

An aircraft auxiliary power unit (APU) was used as an exhaust source for evaluation and refinement of sampling and analytical procedures for gas turbine engines. The unit was also used to determine the emission characteristics of APU's in service and to study the effect of fuel composition and combustor design on exhaust emissions. Carbon monoxide, carbon dioxide, oxides of nitrogen, hydrocarbons, aldehydes, particulate loading, and odor were measured at engine operating modes representing the duty cycle encountered in airline operation. Analyses showed good repeatability, and adequate sensitivity was attained in these experiments. Smoke opacity measurements were not taken owing to the lack of a high-sensitivity smokemeter. Results showed that the minimum emission levels occurred with the standard combustor and Jet A fuel. Emission rates were highly dependent on test mode, but emission patterns as a function of test mode were similar for all fuels and combustors tested. A comparison of three identical design production combustors showed a variation in average emission rates of less than 5 pct.

Jan 1, 1973

By B. J. Scheiner

Silver ores from the Candelaria District, Nevada, and Round Mountain District, Colorado, were investigated mineralogically and metallurgically. Silver minerals of four distinct groups were identified: (1) silver sulfide; (2) argentojarosite; (3) silver contained in the iron oxide; and (4) manganese carbonate-oxide minerals, Electrooxidation and acid-chloride leaching techniques were investigated as means of altering silver minerals, and their effects on subsequent silver extraction were determined. Application of the knowledge obtained from mineral leaching studies resulted in development of a sulfur dioxide-sodium chloride leaching sequence for extracting silver from these types of ores. Silver extractions of 80 to 85 percent were obtained by leaching the ores with a sulfurous acid-sodium chloride system. This was an increase of 9 to 61 percent silver extraction over that obtained by conventional cyanidation techniques.

Jan 1, 1973

By D. E. Anders

Saturated hydrocarbons from 60 selected samples of a 2,300-foot Green River Formation oil-shale core (Piceance Creek Basin, Colo.) were analyzed by gas-liquid chromatography techniques. Emphasis was placed upon the distribution of normal alkanes and 15 key-branched and cyclic alkanes. The latter compounds consisted of the C15, C16, C18, C19, and C20 chain isoprenoids, the 5-a and 5-ß C27, C28, and C29 steranes, three C30 pentacyclic triterpanes, and perhydro-ß-carotene. The results showed definite evidence of maturation of both the n-alkanes and the branched and cyclic alkanes; however, most if not all of the changes were limited to the indigenous soluble extract and were not the result of additional soluble extract generation from the insoluble kerogen. Source material and environmental variations were important factors in some of the observed differences in the branched plus cyclic alkane compositions.

Jan 1, 1973

By C. M. Frost

Crude shale oil prepared by gas-combustion retorting of Colorado oil shale was hydrogenated over a cobalt molybdate catalyst at an operating pressure of 1,000 psig, temperatures of 781° and 761° F, and liquid hourly space velocities of 0.10 and 0.05 Vo/Vo/hr, respectively. The yields of total liquid products and the amounts of nitrogen and sulfur removed were comparable with those obtained at an operating pressure of 3,000 psig and a liquid hourly space velocity of 1.0 Vo/Vo/hr. Approximately 1.5 times as much gasoline was produced at the lower pressure and space velocities.

Jan 1, 1973

By R. S. Fowkes

A study was made by the Bureau of Mines of the penetration of selected granular materials in an unconfined state by wedge-shaped tools having dimensions comparable with the dimensions of the particles composing the materials. The output force for larger particles fluctuated radically. A custom-designed integrator was used to obtain work as a function of depth of penetration in the form of smooth curves. The influence of wedge angle, depth of penetration, penetration rate, entry angle, compaction state, and particle size on the force required and the work performed was ascertained. Empirical equations describing force and work as a function of penetration were obtained for each set of experiments.

Jan 1, 1973

By L. K. Barker

The purpose of this research was to determine how much, if any, improvement would be made by subjecting hydrogenated shale-oil naphtha to a catalytic reforming process. Preselected ranges of temperature and pressure within the commercial reforming ranges were chosen for investigation and other possible variables were held constant. All tests were made with a liquid hourly space velocity (LHSV) of 3 volumes of liquid feed per volume of catalyst per hour (Vf/Vc/hr) and a hydrogen feed rate of 3,000 scf/bbl. Operating temperatures of 850°,875°, and 900° F were used at pressures of 200,400, and 600 psig. The greatest octane improvement in the naphtha was obtained at a temperature of 900° F and pressure of 200 psig. The reformed naphtha had a clear research octane number of 89, a liquid yield of 80 vol pct, and a yield-octane number of 71.1. The data indicate that a higher temperature could have produced a higher yield-octane number.

Jan 1, 1973

By H. L. Gibbs

A portable radon monitoring instrument capable of making on-the-spot measurements of the radon gas content of uranium mine atmospheres was designed and constructed. The monitor was tested in the laboratory and in operating uranium mines. Good correlation was obtained between the monitor readings and radon measurements made on mine atmosphere samples taken in radon bottles.

Jan 1, 1973

By Laurance L. Oden

Titanium-enriched smelter slag produced commercially by Quebec Iron and Titanium Corp., Sorel, Quebec, was evaluated as feed material for a process developed by the Bureau of Mines to prepare rutile. Glass-forming agents including P205, B203, and two binary mixtures were added individually to the as-received and preoxidized smelter slag, and the nonferrous tramp oxides were effectively partitioned into the resulting noncrystalline phase. Iron in the ferrous oxidation state was moderately soluble in the glass of reduced specimens but less soluble under oxidizing conditions. The solubility of iron oxide in phosphate glass exceeded the solubility of iron oxide in borate glass. Effective conversion of titanium oxide to rutile was not achieved in the high-iron commercial smelter slag, and 20 to 30 pct of the titanium remained as pseudobrookite, a mixed iron-titanium oxide.

Jan 1, 1973

By R. K. Koch

The normal spectral emissivities of liquid Ti, V, Zr, Mo, and Pt were determined at the fusion temperatures in an electron-beam furnace using a water-cooled copper hearth. The normal spectral emissivities were estimated above the melting points by using adjusted two-color temperatures as approximations of the true temperatures for substitution in Wien's equation. Simultaneous brightness temperatures were determined with a micro-optical pyrometer. The true temperature ranges covered were 1,668° to 1,885° C for Ti; 1,919° to 2,013° C for V; 1,855° to 2,367° C for Zr; 2,610° to 2,751° C for Mo, and 1,772° to 1,990° C for Pt. The spectral emissivities for titanium and zirconium decreased with increasing temperature. At an effective wavelength (?) of 658 mµ the emissivity of titanium ranged from 0.51 to 0.45 and zirconium, from 0.47 to 0.41. The emissivities of vanadium (? = 658 mµ) and molybdenum (? = 657 mµ) were constant at 0.41±0.02 and 0.33±0.01, respectively. The spectral emissivity of platinum (? = 658 mµ) was constant at 0.39±0.02 up to 1,900° C; above that temperature anomalous data were obtained. A mass spectrometric study indicated that platinum was reacting with back-streaming silicon vapors from the diffusion pump when the ambient pressure was greater than 2 X 10-5 torr.

Jan 1, 1973

By Ronald A. Munson

Samples of the naturally occurring zeolites phillipsite, clinoptilolite, erionite, and chabazite have been surveyed for their gas adsorption, ion exchange, and other characteristics. Chabazite and erionite, which are generally more stable, also have higher methane adsorption capacities than do the other natural zeolites. Both natural erionite and natural chabazite are classified as small-port zeolites on the basis of their inability to adsorb chlorotrifluoromethane. In the range of 8 to 100 mesh, the adsorptive capac-ity of natural zeolites is improved only slightly by a decrease in particle size. The capacity of natural clinoptilolite to adsorb methane is increased by cation replacement by the hydrogen ion and decreased by exchange with calcium ion. Natural phillipsite, which is easily decomposed by heat, adsorbed methane to a limited extent.

Jan 1, 1973

By A. R. Rule

Research was conducted by the Bureau of Mines to develop a process for utilization of Idaho kyanite. A continuous gravity-flotation separation process was applied successfully to recover kyanite-group minerals from an Idaho ore containing about 21 percent combined kyanite, andalusite, and sillimanite. Dry magnetic separation of the concentrate resulted in a product containing about 90 percent kyanite at a recovery of 63 percent of the kyanite-group minerals in the ore, Alumina and silica analyses were within the range generally accepted for conversion to mullite, and the finished products had a pyrometric cone equivalent of more than 38. A recovered garnet coproduct may be of commercial value.

Jan 1, 1973

By Foster Fraas

This report describes the application of pulsed magnetic fields derived from alternating and intermittent magnetizing currents. Application of such pulsed magnetic fields to the matrix-type separator permits (1) the complete discharge of the magnetic fraction with wet feeds and (2) the dry separation at particle sizes down to 325 mesh. At smaller particle s indications are that frequencies above 60 hertz will be required. Applications of intermittent magnetizing current to the cross-belt separator give the cross-belt-separator an advantage over the conventional constant-field cross-belt and induced roll separators; the intermittent current enables the cross-belt separator to separate matted fibrous and magnetically coagulating feeds, a type of feed that occasionally occurs with mineral, industrial, and secondary materials.

Jan 1, 1973

By D. G. Kuehn

Mass spectrographic studies have been conducted on the positive ions and neutral species of glow discharges containing 1.0 pct S02 and 1.0 pct CO in helium. Measurements were conducted for gas pressures from 3.5 to 10.1 torr using both dc and 60-Hz ac excitation. The ion species that were observed included S+, SO+, SO+, 0+, O2+, C+, CO+, and CO2+ with lesser amounts of SO3+, (CO)2+, SCO+, and (SO?CO)+ or CS+2. Interpretation of the functional dependence of the various ionic and neutral species on pressure and applied power showed that CO reacted with the SO formed in the discharges to produce CO2 and sulfur. Deposition of elemental sulfur was observed in the plasma container.

Jan 1, 1973

By Lewis V. Wade

This Bureau of Mines work was performed to theoretically determine the effects of specimen radius and specimen boundary conditions on the stress state in the rock near the anchor for rock specimens used to investigate expansion anchor behavior. Finite element analyses were performed on mathematical models of varying radius and boundary conditions. A review of the results of these analyses revealed a definite convergence of all stress measures considered as the specimen radius increased. There was, however, a significant variation in all stress measures as the specimen diameter increased from 8 to 12 inches.

Jan 1, 1973