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By P. R. Tisot

Structural response and/or deformation was determined for each of four different grade Green River oil shales (27.0-, 34.5-, 45.5-, and 63.5-gal/ton) as they were heated in an inert atmosphere, under constant compressive stress, from ambient to subretorting temperatures; that is, below those required for rapid pyrolysis of the organic matter. Small cores and small columns of confined fragments comprised the test specimens, which were heated, in a specially designed microunit, at a uniform rate either to 725° or to 825° F under three different stress levels, 80, 200, and 325 psi. Structural response of some cores was observed as they were heated in a stress-free environment. The obtained stress-strain-time-temperature relationships provide information regarding the oil shale's yield temperature, yield stress, rate of compressive strain, loss of mechanical strength, and nature of structural deformation. Effects of structural deformation on induced permeability in small columns of fragments are presented. Results indicate that underground retorting of Green River oil shale may be seriously impaired through loss of induced permeability brought about by structural deformation of rich oil shale under the influence of heat and compressive stress.

Jan 1, 1971

By T. A. Sullivan

The processing of sweated aluminum electronic scrap was investigated to develop methods for recovering the aluminum and concentrating the other metals, including copper, lead, gold, and silver, into a product that can be separated by known methods. Two molten-salt electrorefining processes were developed and tested. The first process utilized a three-layer refining cell with a BaCI2-NaF-AIF3 electrolyte, which operated at 750° to 850° C. The second process used an all-chloride electrolyte of NaCI-KCI-AICI3 at 750° to 800° C, with separate anode and cathode compartments. High-quality aluminum was recovered that averaged 99.8-percent pure in the three-layer cell and 99.6-percent pure in the compartment cell. Over 94 percent of the aluminum was recovered with cathode current efficiencies of approximately 90 percent in both methods. The copper, lead, tin, silver, gold, and other metals were concentrated threefold in an anode product. Separation of lead and part of the tin by liquation from this product seemed feasible. The anode product was smelted to prepare a 96-percent copper bullion that contained 690 ounces of silver and 65 ounces of gold per ton, with 98 percent recovery of these values.

Jan 1, 1972

By William J. Campbell

Three types of X-ray analytical instrumentation were compared for applications in the secondary brass and bronze industry. The instruments were a conventional X-ray spectrograph, a portable X-ray spectrograph, and a radioiso-topic X-ray analyzer using balanced filters. The following two general applications were considered: Rapid identification for sorting scrap metals and quantitative analyses to provide guidance in the melting and casting of alloys. Twenty-three analyzed copper-base alloys were used as standards. Although the alloys varied widely in composition, matrix correction procedures were not necessary except for copper. The conventional X-ray spectrograph provides positive identification of the alloys and quantitative values for the six elements investigated--aluminum, copper, iron, lead, tin, and zinc. Equivalent results were obtained with the portable X-ray spectrograph for those elements whose characteristic X-rays are in the wavelength range of the instrument. The radioisotopic X-ray analyzer distinguishes certain groups of alloys and provides quantitative determinations for copper, lead, tin, and zinc. The sensitivity of the analyzer was marginal for the determination of small concentrations of elements of atomic number 26 or lower.

Jan 1, 1972

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 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 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 C. M. McCulloch

A geologic study of Mines 32 and 33 in Cambria County, Pa., was conducted as part of a methane control research program. Areas of high methane emission and roof instability are encountered which are related to the structural and stratigraphic features that characterize the geologic setting of these mines. Locally the folds trend N 20° E ±2°, the direction of the butt cleat in the Lower Kittanning coal. The face cleat strikes at N 69° W ±2° and the systematic rock joint in the surface bedrock strikes N 67° W ±2°. This suggests that a directional stress oriented N 70° W produced the folds and influenced the directions of coal cleat and systematic joint sets. Analysis of SLAR indicates three directions of prominent regional lineation: N 39° E, N 31° W, and N 70° W. Little gas was encountered during development mining; large volumes of gas are encountered when roof falls. Most of the gas comes from strata above the mined coal; therefore, to control methane, roof instability must be controlled. Roof falls and high rates of methane emission are most likely where less than 30 feet of many thin layers of limestone, shale, and sandstone occurs between the Lower Kittanning coal and the next coal and in zones along the margins of a sandstone channel.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By M. Hertzberg

Results of a comprehensive study of the absolute spectral radiance of the infrared emissions from methane-air explosions are reported. The spectral growth of these expanding flames were recorded with a time resolution of 1 msec in the spectral range of 1.7 to 5.0 µm. Time-resolved spectra were obtained for methane-air mixtures as a function of stoichiometry, nitrogen dilution, and Halon dilution, in a 9-liter vessel under different venting conditions. Data are also presented for coal dust-air explosions. Temperatures, obtained from the absolute radiances and from a band ratio technique for methane-air, are internally consistent and are generally 50° to 200°K below adiabatic flame temperatures. All near limit mixtures gave essentially the same flame temperatures (1,500° to 1,600° K) regardless of whether the limit was obtained by dilution with excess air, excess methane, excess nitrogen, or Halon. The coal dust explosion spectrum is essentially a blackbody continuum at 1,500° K with some selective emission at 4.4 µm from hotter CO2. The data are analyzed in terms of the radiative dynamics of a sperically expanding flame zone. The importance of radiative transport is assessed. An equation is derived which relates the instantaneous fraction of combustion power radiated to adiabatic variables.

Jan 1, 1973

By H. B. Carroll

This Bureau of Mines report evaluates the performance of commercially available portable instrumentation for the detection of carbon monoxide, carbon dioxide, oxygen, and methane at conditions simulating an industrial work atmosphere. Portable instrumentation included in the study was gas-detection tubes (length-of-stain and color intensity), catalytic detector, liquid absorption detectors, paramagnetic oxygen detector, galvanic detector, and pelement or hot-wire methane detectors. Evaluation of the instruments was in atmospheres with 50 and 80 percent relative humidities at 75° F and containing test gas concentrations of 0.1, 0.25, 0.50, 1.0, 1.5, and 2.0 times the thresh-old limit value. Correlation of the results from the portable gao analyzer with measurement from the standard instruments was made by calculating and plotting an estimated line of regression, prediction, and confidence limits and the correlation coefficient for each detector system. Relative humidity in the 50-to 80-percent range did not appear to contribute to instrumental uncertainties in either performance or operation. Considerable deviation in detection precision between the portable gas-detection systems and the standard systems was established, especially at the lower gas concentration levels. The main difference or inconsistency in toxic gas concentrations determined with length-of-stain tubes resulted from the observer's interpretation of the results rather than difference in the tubes themselves.

Jan 1, 1973

By J. S. Miller

This report presents a complete coverage of results from Bureau of Mines preliminary research and the field application of explosive fracturing techniques to prepare oil shale for in situ recovery of shale oil. Small-scale surface tests were conducted to determine the feasibility of using a nitroglycerin-base explosive for creating rock fractures. Prior to underground testing, surface and near-surface tests with liquid explosives showed that explosions in sheetlike layers simulating underground fractures would propagate effectively. Successful surface experiments were conducted using layers of explosive placed between glass plates and explosive-saturated sand confined in small-diameter metal tubes. The tests in glass-plate reservoirs and metal tubes demonstrated that nitroglycerin would detonate and the explosion would propagate in cracks as thin as 1/32 inch and through distances up to 12 feet. In a shallow field test, nitroglycerin was detonated in a vertical crack in limestone and produced extensive fracturing. Explosive fracturing tests were performed in oil shale formations on seven sites near Rock Springs, Wyo. The procedures included (1) displacing and detonating nitroglycerin in natural or hydraulically induced fracture systems; (2) detonating nitroglycerin in wellbore shots; (3) displacing and detonating nitroglycerin in induced fractures followed by wellbore shots using pelletized TNT; and (4) detonating wellbore charges using pelletized TNT. The research on oil shale formations demonstrated that nitroglycerin displaced in a natural or hydraulically induced fracture would detonate, and the explosion would propagate through the explosive-filled fracture. Shooting a pattern of wells in oil shale at 100-foot depth with wellbore charges of pelletized TNT developed a satisfactory interwell fragmented zone. Tests performed on other sites at depths to 385 feet caused fragmentation of rock around the wellbore and provided interwell communication. Fourteen methods used to evaluate the extent and degree of fragmentation in the explosive fractured oil shale are discussed.

Jan 1, 1974

By Russell E. Griffin

Dielectric constants and dissipation factors were measured by the Bureau of Mines for 13 simulated lunar rocks over the 20-to 100-megahertz frequency range by means of the susceptance-variation method. Measurements were made at room temperature and normal atmospheric pressure. Results are presented and some comparison is made with data reported by others. The rocks used include a broad range of physical characteristics and chemical compositions from the large areas of volcanism in Oregon and northern California, and two nonvolcanic types. These rocks make up a suite of rock standards used by a group of laboratories engaged in lunar research. The data presented will add to the basic scientific and engineering knowledge needed to utilize extra-terrestrial mineral resources for support of future space missions.

Jan 1, 1974

By C. Daniel Kealy

Dissolved and suspended solids are present in the free water of tailings ponds. This Bureau of Mines study was designed to identify the influences of the slime zone in preventing these solids from reaching the environment outside the tailings pond. The finite-element method was used to determine the rate of discharge of subsurface water from the Van Stone tailings pond in northern Washington. The slime zone was sampled and tested for the first time, and results were interpreted and incorporated into the mathematical model. Computer results were verified by installing and monitoring piezometers in the field and by a simulated (16- by 1/2- by 3 foot) laboratory model. Output from the numerical model defined critical seepage zones and revealed that proper pond design and maintenance can reduce pond seepage losses to a minimum. Minimization of seepage requires maintaining the pond water level over the slime zone. Sufficient physical, chemical, and limnological data were collected and analyzed to conclude that the only realistic reflection of synergistic effects is obtained by study of the indigenous biota in combination with quantitative chemical and physical data. Proper planning and management of the milling and waste disposal operations are the key to minimal pollution.

Jan 1, 1974

By Z. J. Fink

Ultraviolet-visible and infrared emission spectra from propagating methane-coal-dust-inhibitor mixtures have been obtained in a 0.2-by 0.2¬by 5.3-m vertical duct over a range of flame speeds from 2 to 100 m/sec. Results serve as a basis for the design and evaluation of thermal radiation detectors for triggered barriers that suppress ongoing mine explosions. Of particular significance is the large continua superimposed on the methane-air spectra when small amounts of coal dust are present and the variation of emissivity with infrared (IR) wavelength in dust flames. In conjunction with the spectral measurements, studies of flame speed, particle size, gas sampling plus thermodynamics, and dust sampling are presented and discussed in order to gain insight into the more fundamental aspects of propagating explosions. Sampling results have shown that only a near-stoichiometric amount of dust is consumed in the flames studied even though initial concentrations are five times stoichiometric. Difficulty in propagating coal-dust inhibitor flames of realistic mine characteristics in a cold-walled laboratory duct has been encountered. A simplified analysis of the flame zone utilizing spectral and sampling results indicates that the stability of slowly propagating flames is more dependent upon thermal radiation than upon convection losses to the walls. It is predicted that thermal radiation losses will make any measurements of coal dust burning velocities, "quenching diameters," or flammability limits more apparatus dependent than those corresponding to gaseous fuels.

Jan 1, 1974

By Eugene H. Skinner

This Bureau of Mines report describes the fieldwork and subsequent analysis to determine physical properties, stress distribution, and several aspects of rock behavior as a necessary evaluation for a typical mine opening. All work was done at a test site on the 3300 level, Crescent mine, Coeur d'Alene mining district, Idaho. Free field stress beyond the influence of the opening was also determined. Conventional overcore technique with the three-component borehole deformation gage developed by the Bureau of Mines was used in three drill holes. Three field verification tests were performed using a gage newly developed by the Spokane Mining Research Center in an approach herein termed "initial deformation method." Use of this method validated that aspect of overcore theory which predicts that similar deformation effect occurs in the wall rock around the perimeter of an opening in rock under stress. Also described are all drilling procedures and performances. Physical property determinations were made on rock samples obtained from the three overcore drill holes. Twelve physical properties with a total of [532] values were obtained at various drill hole orientations and depths. Exhaustive statistical tests were utilized in the analysis of these physical properties. Further elaborated are statistical inferences based on these analyses. Extensive analysis and interpretation of Crescent mine geology are also described.

Jan 1, 1974

By Richard A. Busch

Inadequate engineering design criteria for coal refuse embankments has allowed hazardous impoundment structures in coal mining areas to be created. A necessary first step to develop adequate design criteria is the determina¬tion of basic, respresentative physical property data on the materials that constitute typical refuse embankments. An extensive field and laboratory program was undertaken by the Federal Bureau of Mines. Much physical property data was generated. Additonal petrographic analysis and large scale triaxial compression testing was performed by others. The data presented here should aid in establishing design parameters for coal refuse embankments

Jan 1, 1974

By E. S. Shedd

Amenability studies were conducted by the Federal Bureau of Mines on an electrooxidation technique for the extraction of mercury from cinnabar ores, particularly those that are too low in grade to be furnaced or retorted economically. Oxidation was accomplished by electrolysis of the ore while slurried with brine. Mercury was dissolved through the formation of the soluble tetrachloro mercury complex, HgC142-. Mercury extractions ranged from 90 to 98 percent in 4 to 6 hours of processing time when tests were made on eight different types of cinnabar ores containing from 0.7 to 18 pounds mercury per ton ore. Salt concentration was varied from 4 to 10 weight-percent depending on whether Pb02 anodes and iron cathodes were used or whether graphite was used for both electrodes. Power consumption ranged from 17 to 64 kilowatt-hours per ton of ore treated. Ninety-nine percent of the mercury was recovered from pregnant solutions by precipitation on an active metal such as zinc, followed by distillation of the resulting amalgam at 600° C.

Jan 1, 1975

By Michael L. Boucher

Copper and nickel sulfides occurring in the Duluth Complex of northern Minnesota were examined at the Bureau of Mines, A microscopic study was undertaken to determine the mineralogy and paragenesis of the ore minerals. Eighty-two samples were taken from one deep diamond drill core located near Babbitt, Minn. Modal analyses are presented for the Duluth Complex rocks and for the are minerals in the major mineralized zone. The major sulfide minerals are chalcopyrite, cubanite, pyrrhotite, troilite, and pentlandite. Results of this investigation suggest that the mineralization is related to the structural features of the enclosing rocks: pores, open fractures, and cavities. The pyrrhotite-troilite-pentlandite assemblage is believed to have formed from an immiscible sulfide melt, probably associated with the troctolitic rocks. Most of it settled to the very porous base of the Duluth Complex, and to the other porous zones near xenoliths; small portions were trapped higher in the section. A later introduction of a copper-rich sulfide melt replaced some of the pyrrhotite-troilite and oxides, and filled in the remaining open spaces and fractures in the Duluth Complex and those of the adjacent footwall rock.

Jan 1, 1975

By Joan T. May

The Bureau of Mines conducted laboratory tests to evaluate the production of high-purity H3P04 by HCl digestion and solvent extraction. Both batch and bench-scale continuous tests were made. Western phosphate rock concentrates were acidulated with HCI, and the digestion liquors were processed by solvent extraction. Phosphoric acid was extracted with isoamyl alcohol and recovered from the organic extract by contact with an NH4F solution. This solution was fractionally distilled to yield high-purity H3P04. The raffinate from solvent extraction was treated with lime to precipitate CaF2, which was subjected to steam pyrolysis to generate HF. This method was successful in recovering 95 pet of the phosphate and 80 pct of the fluoride contained in the concentrates.

Jan 1, 1976

By Michael J. Beus

This Bureau of Mines report describes a tunnel stress relaxation gage (TSR) developed to measure initial radial displacement around full-sized underground openings. The TSR technique was shown to be a valid concept in previous field verification tests. Sensitivity has been improved by employing a titanium alloy cantilever in the transducer head, which also permits a deeper sensor location. Use of improved fabrication methods such as stainless steel bellows and sputtering techniques and use of an environmental chamber for testing greatly increased overall reliability. A miniature data acquisition system (DAS) was interfaced directly to the transducer for increased versatility and containment entirely within a borehole. The present TSR system is suitable for use around full-size underground excavations, particularly machine-bored openings. Field evaluation of the improved instrumentation verified the design goals.

Jan 1, 1978