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By O. Q. Leone

A processing unit was developed for the complete cleaning of titanium alloy chips. The process uses solvent degreasing, magnetic separation, and anodic solution of nonmagnetic impurities in 10 weight-percent sulfuric acid. Vacuum arc-melted ingots weighing approximately 10 pounds each were prepared from cleaning chips according to ingot specifications.

Jan 1, 1973

By J. B. Janus

This report, the 22d in a series, gives analytical data showing composition and quality of tipple and delivered samples of coal collected during fiscal year 1972. This coverage lists mines located in 20 States. Ultimate analyses are given for most of the coalbeds listed. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. The deliveries were sampled in accordance with instructions issued by the Bureau of Mines, and the samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1973

By R. Blickensderfer

The sparking and gas-igniting tendency of steels and alloys were evaluated my measuring the radiance of spark showers produced by grinding a sample on an abrasive wheel in air, the time required for a spark shower generated on an abrasive wheel to produce an ignition in an explosive gas mixture, and the energy and speed required for impacts between various materials to ignite an explosive gas mixture. Mixtures of air-methane were found quite resistant to ignition by showers of sparks. A mixture of air-9.S pct hydrogen was used to increase the sensitivity of the tests and to thereby extend the range of materials that could be evaluated. The results of the spark-shower tests indicate that carbon steels and the alloy steels found in coal-cutter tools are among the most sparking and most incendive of any materials tested. Stainless steels, nickel alloys, and tungsten carbide are among the least sparking and least incendive. The brightness of the spark showers depended upon the degree of oxidation of the abraded particles. Impact tests against hard rocks such as solid quartz and sandstone, showed that high-carbon steel was more inc endive in the hydrogen mixture than were the softer steels or the alloy steels found in coal cutters. Ignitions were found much less likely to occur at speeds somewhat lower than the speeds currently in use in continuous mining machines.

Jan 1, 1972

By T. Kessler

As part of a respirable mine-dust research program at the U.S. Bureau of Mines, spark-source mass spectrometry has been used for the semiquantitative determination of trace elements (200 ppm weight or less) in raw coals. In addition, several minor and major elements have been determined using this technique. Sixty-four elements ranging in concentration from 0.01 to 41,000 ppm weight were determined in one anthracite, two mvb, four lvb, and six hvab raw coal samples. The samples represented 10 coal seams located in Pennsylvania, West Virginia, Virginia, Utah, and Colorado.

Jan 1, 1973

By M. A. Mahtab

This report presents the geometric parameters (attitude, spacing, extent, and aperture) of fracture patterns in a selected portion (study area) of San Manuel copper mine, Arizona. The geometric parameters are quantified for input to structural analyses for studies of the influence of fractures on cavability of ores. Using an orientation analysis procedure developed earlier by the Bureau, three prominent and nearly orthogonal sets of fracture orientations were delineated in the study area. Sets 1 and 2 dip nearly vertically, and generally strike east-west and north-south, respectively, whereas set 3 is nearly horizontal. Both a horizontal rotation (of 14° to 26° for sets 1 and 2, respectively) and a tilt (of 20° for set 3) is shown to occur between the 1415 and 2015 levels of the mine. Gomparison of the three major rock types present in the study area (quartz monzonite, monzonite porphyry, and rhyolite) show that the rhyolite is characterized by short extent, small spacing, and tightness of fractures as well as the general absence of fracture set 3, which may account for its generally observed strong resistance to caving.

Jan 1, 1973

By E. G. Valdez

Three cryogenic systems that utilized liquid nitrogen, dry ice, and methanol with dry ice were investigated in conjunction with crushing and classifying techniques. The systems were used to aid in separating and reclaiming the metallic components contained in insulated wires, shredded automobile nonferrous metal concentrates, small motors, generators, and rubber tires. Wire strands, 2 to 6 inches long and insulated with polyvinyl chloride and neoprene, were chilled at -60° and -195° C, then roll-crushed and processed by water elutriation; this procedure resulted in two products--a sink fraction that was 99 percent metallic and a float fraction that was 99 percent nonmetallic. Excellent separation of zinc die-casting alloys from copper and aluminum contained in shredded automobile nonferrous metal concentrates was attained by chilling at -72° C for 1 minute, crushing in a grateless hammer mill, and screening. From the screened products, 97.2 and 100 percent of the copper and aluminum, respectively, were recovered in the plus Pinch fraction, and 100 percent of the zinc was recovered in the minus 1-inch fraction of over 97 percent zinc die-cast purity. Laboratory experimental results comparing direct and indirect chilling indicated that a sufficiently low temperature could be attained by indirect chilling to permit use of a liquid C02-dry ice system on insulated wires and mixed nonferrous metallic concentrates.

Jan 1, 1973

By M. J. Kovalik

Illinois No.6, a high-volatile B coal of low fluidity, was blended with fluidized-bed char and coke breeze to improve the strength of the coke obtained from carbonizing this coal. Twenty-one tests, selected from those made in the small-scale Hanson carbonizer, were carbonized in the BM-AGA 13-inch-diameter, cylindrical retort, with a coal charge of about 90 pounds; the strength of the cokes was determined by the standard ASTM tumbler test. Using the same procedure, 10 tests were made with High Splint, a high-volatile A coal from Harlan County, Ky. Carbonization of the blends produced larger and stronger cokes than did the Illinois No.6 coal singly. The optimum blend contained 6 percent each of char and coke breeze. Further improvement in coke strength was realized by either preheating this blend prior to carbonization or by adding a small pro-portion of a premium blending coal. The former method could possibly eliminate the use of premium coking coals in blends with Illinois No. 6 coal to make an acceptable metallurgical coke. Except for no improvement in coke strength by preheating, results for High Splint coal showed behavior similar to that of the Illinois No.6 coal.

Jan 1, 1973

By E. Aamland

Preparation of high-purity magnesium-yttrium alloys by electroreduction of Y2O3 dissolved in a YF3-LiF bath and the subsequent deposition of yttrium in a molten magnesium cathode was investigated in laboratory-scale apparatus. Parameters such as temperature, current density, and electrolyte density were studied. Electrolysis was conducted in a specially designed MgO diaphragm cell at temperatures ranging from 780° to 970° C. Alloys containing up to 55 weight-percent yttrium were prepared at cathode current efficiencies of 21 to 60 percent. Cell design and operation are described, and some of the limiting conditions pertaining to the method are discussed.

Jan 1, 1973

By Joan C. Biordi

A molecular beam-mass spectrometer-low pressure flat flame apparatus has been constructed for the purpose of examining the chemical microstructure of normal methane-oxygen-argon flames and those inhibited with Halon extinguishants. Details of construction and performance of this apparatus and of related flame temperature measurements are given. Particular attention is paid to the empirical characterization of the perturbation to the flame caused by the sampling probes. The composition profiles obtained for normal flames are compared to those of flames inhibited by CF3Br. In addition to the usual stable species (CH4, O2, CO, CO2, H2O, H2, and H2CO), the inhibitor, its products and intermediates associated with its reactions could be followed. In particular, hydrogen bromide, bromine atoms, hydrogen fluoride, and carbonyl fluoride were observed. The relatively rapid disappearance of inhibitor and early appearance of fluorinated reaction products suggest a short lifetime for the CF3 radical in this system. Observation of COF2 suggests that CF3Br is effective as an inhibitor, at least in part, by virtue of its interference with the oxygen containing species of the normal chain reaction. Profiles of the 17+ peak at low electron energy suggests that the hydroxyl radical may also be sampled, but the profiles obtained are not yet sufficiently accurate to determine the effect of inhibitor on this important flame radical.

Jan 1, 1973

By K. J. Liles

The Bureau of Mines conducted laboratory semicontinuous and continuous heavy liquid tests to determine the feasibility of producing commercial-grade products from the high-clay sylvinite ores of the Permian Basin in New Mexico. Continuous test operations demonstrated that concentrates containing 59.9 percent K2O and recoveries of over 75 percent of the contained potash can be obtained. The organic heavy liquid was effectively recovered by vaporization, condensation, and absorption methods. Less than 5 parts per million of heavy liquid vapors were released to the atmosphere. This loss represents only 0.02 pound of heavy liquid per ton of ore treated.

Jan 1, 1973

By R. C. Wang

Solid-liquid flow in different pipe geometries was investigated. This investigation was conducted by measuring delivered solids concentration and head loss. The delivered solids concentration was measured to study the effect of pipe geometry on the minimum carrying velocity above which solids do not lag behind the fluid. Head loss was measured to study the effect of pipe geometry on the friction loss. A mathematical formula was developed for determination of the minimum carrying velocity. Darcy-Weisbach's equation and Durand's equation were used for comparison of head losses of pipe shapes. Of the different pipe shapes studied, each having the same interior cross-sectional area, the rectangular pipe with the wide side oriented as the base yielded the lowest minimum carrying velocity at high solids concentrations. The minimum head loss at low velocity and high solids concentration also was attained with this pipe. Although the circular section is known to be the best for transporting liquid only, the present study suggested that pipe geometry is a factor in lowering the operating velocity and reducing head loss in solid-liquid flow.

Jan 1, 1973

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 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 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 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