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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

By F. E. Joyce

This paper describes the development of a process for producing manganese and iron pellet concentrates from low-grade manganiferous iron ores of the Cuyuna range by a two-stage sulfatization-reduction roast. First, the manganese minerals (7.5 percent manganese) were converted to water-soluble manganese sulfate by roasting in sulfur oxide gases at 700° C, then, the hematitic iron minerals (31 percent iron) in the hot sulfatized are were reduced to magnetite with simulated reformed natural gas in the temperature range of 350° to 425° C. Batch tests were made in a 3-inch-ID by 6-inch-long, gas-heated, stainless steel retort, and continuous countercurrent experiments were performed in a 2-inch-ID by 10-foot-long, electrically heated shaft furnace. Manganese sulfate was removed from the roasted product by leaching with water, and over 90 percent of the manganese was recovered in an oxide product (65 percent manganese) obtained by precipitation, drying, and thelmal decomposition of the sulfate. An iron oxide concentrate (60 percent iron) with an iron recovery of 75 percent was obtained from the water-insoluble residue by magnetic separation.

Jan 1, 1973

By B. J. Scheiner

The Bureau of Mines investigated an electrolytic technique for oxidizing ore slurried with brine to determine its effectiveness in extracting mercury from ores. Optimization experiments conducted on a 2.5-pound-mercury-per-ton ore resulted in 95 percent mercury extraction with operating conditions of 30° C, a current density of 0.5 ampere per square inch, and a treatment time of 3.5 hours. Corresponding power consumption amounted to 38 kilowatt-hours per ton of ore treated. Amenability experiments conducted on 62 different mercury ores resulted in 90 to 99 percent mercury dissolution from ores containing 0.6 to 20 pounds of mercury per ton of ore, Treatment time ranged from 1 to 7 hours in 4-to 20-percent sodium chloride solutions, and power consumption was in the range of 10 to 50 kilowatt-hours per ton of ore. Pilot mill experiments in a 100-to 200-pound-per-hour extraction plant have been in progress to quantify power and reagent requirements. These data will be reported in a subsequent publication.

Jan 1, 1973

By James J. Olson

The Bureau of Mines used micro fracture density analysis of quartz grains in thin sections and diametric pulse velocity measurements along preblast and postblast cores to determine the nature and extent of rock damage produced by small (0.25-,0.50-,1.0-, and 2.0-kg) charges of high intensity explosive (C-4) in granite. Pulse velocities from the postblast cores were significantly lower than velocities from the preblast cores and, with the core logs, provided clear identification of the upper and sometimes the lower limits of most severe damage. These zones ranged from about 1.68 ft for the 0.25-kg blast to 4.16 ft for the 2.0-kg blast. Microfracture densities from postblast cores were significantly higher and more variable than densities measured from preblast cores. The microfracture density measurements showed that microscopic damage was present far past the zones of most severe damage as delineated by the pulse velocity logs and core logs. An exponential relation-ship was observed between the micro fracture density levels and the charge weight.

Jan 1, 1973