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By John Ward Smith

Aragonite, co-occurring with calcite and dolomite as matrix minerals, has been discovered in Mahogany zone oil shales of Colorado's Eocene Green River Formation, posing puzzles on the geochemical patterns of their separate origins, reasons for their simultaneous existence, and their interrelation. The presence of aragonite is demonstrated by X-ray diffraction. Amounts of aragonite and dolomite are significantly and inversely related, but the calcite quantity is essentially independent of either aragonite or dolomite quantity. A geochemical pattern outlining the deposition conditions that created the Green River Formation oil shale is postulated from characteristics of the oil shale. The development of the three separate carbonates--aragonite, calcite, and dolomite--the inverse relationship between aragonite and dolomite, and the independence of amounts of calcite and the other two carbonates are shown to be natural consequences of this oil-shale genesis pattern.

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 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 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 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 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 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 D. S. Burgess

This report summarizes the incidents that preceded the December 9, 1970, propane-air explosion in Port Hudson, Mo., and then attempts to establish the nature of the explosion from the ensuing events. Special emphasis is given to possible ignition sources, the distribution of flammable vapors, and the analysis of blast damage. Both near-and far-field damage indicated that this explosion may be attributed to the detonation of propane in air with an energy release equivalent to that from about 50 tons of detonating TNT.

Jan 1, 1973

By David E. Siskind

The Bureau of Mines has studied the fracturing and associated damage occurring in the vicinity of blastholes from five shots fired in the shale pillars in the White Pine copper mine, White Pine, Mich. Four types of explosives (AN-FO, commercial extra dynamite, ammonia gelatin dynamite, and a low-density, low-velocity permissible) were used. Cores were taken from the blast region and examined by ultrasonic and petrographic techniques. Pulse wave velocities were measured across the core diameters, and thin sections showing cracks and changes in lithology were examined in an attempt to establish zones of damage. Cores from the blast regions and areas near pillar free faces were found to have abnormally low pulse velocities. Petrographic study of the thin sections showed that the negative velocity anomalies were caused by cracks in the cores. Crushing and extensive fracturing prevented meaningful measurements on core fragments from the immediate blast vicinities. Compositional, changes and other rock nonuniformities, such as joints and preexisting fractures, tended to mask detailed damage differences among the four explosives; however, the two most energetic explosives (extra dynamite and ammonia gelatin dynamite) produced damage zones two to three times as large as the AN-FO and low-velocity permissible explosives.

Jan 1, 1973

By H. E. Powell

This Bureau of Mines study describes two processes for recovering zinc, copper, silver, and iron from the magnetic fraction of a waste generated by the primary smelting of zinc in horizontal retort distillation furnaces. The laboratory-scale procedures include reduction melting to produce a high-copper iron and matte smelting to produce a copper-silver-iron matte and metallic iron. Zinc is fumed in each process and recovered as the oxide. Direct reduction melting yields a metallic iron high in copper and a small rich matte from the sulfur contained in the waste. The products of the second process are a matte containing essentially all of the silver, about 80 pct of the copper and 37 pet of the iron, and an iron-copper alloy containing all of the remaining copper. Extraction with metallic lead or sodium sulfate recovers essentially all of the copper from the molten high-copper iron and yields an acceptable foundry iron.

Jan 1, 1973

By Paul J. Barrett

The Bureau of Mines evaluated a sulfurous acid-sulfuric acid process for recovering alumina from clay, in which clay is leached. successively with sulfurous acid and sulfuric acid. The resulting aluminum sulfite and aluminum sulfate solutions are combined and heated to produce a basic aluminum sulfate and sulfur dioxide. Alumina is extracted from the basic aluminum sulfate as sodium aluminate by leaching with dilute sodium hydroxide. After desilication, sulfuric acid is used to precipitate alumina as alumina trihydrate, which is then calcined to alpha-alumina. The estimated fixed capital cost for a plant producing 1,000 tons per day of alumina is about $74 million on a 1971 basis. For comparison with previous alumina-from-clay evaluations, the estimated fixed capital cost for the plant is about $67 million on an M and S Chemical Equipment Index basis of 24.0.0, which is equivalent to a 1960 cost level. Because the operating cost is highly dependent on fuel and electric power costs, graphs are included to show the effect of these items on the operating cost. On a 1971 basis, with natural gas costing 35 cents per million Btu and operating labor costing $4 per hour, the estimated operating cost is about $100 per ton of alumina. On a 1960 basis, with labor costing $2.30 per hour and natural gas costing 25 cents per million Btu, the estimated operating cost is about $86 per ton of alumina.

Jan 1, 1973

By Byron A. Baker

The Bureau of Mines used a windowed cell to measure the phase-boundary pressures of two related series of gas-condensate fluid mixtures. Normal butane was added to the mixtures incrementally to determine its effectiveness for lowering phase-boundary pressure. All the experimental data were correlated, so that the pressure required to maintain light oils mixed with natural gas in the single phase may be computed for secondary recovery applications. The heavy hydrocarbon parts of the mixtures were distillation fractions of a Gulf Coast condensate. Intermediate normal hydrocarbons in the butane-heptane range and natural gas were added to the fractions in selected proportions, so that phase-diagram pressures of 26 fluids were actually studied. The experimental range of temperatures was 50° to 280° F. Two correlations were developed to represent phase-boundary pressures by means of a polynomial. Independent variables represent natural gas content, disparity of properties of components comprising the mixtures, and temperature. A fourth variable, for one correlation only, was the quantity of normal butane added to the original mixtures. The latter correlation with four independent variables contains 15 coefficients and is estimated to be accurate to 135 psi.

Jan 1, 1973

By P. M. Sullivan

At its College Park Metallurgy Research Center in Maryland, the Bureau of Mines has installed and is operating a 5-ton-per-hour pilot plant for continuous mechanical separation of values contained in raw urban refuse. The entire sys tern was assembled using commercially available equipment. The process relies on multistage processing including shredding, air classification, screening, gravity concentration, and electrostatic separation. Compactor trucks deliver raw refuse collected along typical routes in metropolitan Washington, D.C., to the pilot plant. The loads are separated into concentrates of (1) light-gage iron, (2) massive metals, (3) glass, (4) putrescibles and waste combustibles, (5) paper, and (6) plastics. While some refinements remain to be made in the processing system flow-sheet, the data obtained to date have been highly encouraging, indicating favorable economics for commercial-size plants.

Jan 1, 1973