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By G. H. Keith

Electrowon tungsten powders were investigated with respect to consolidation, fabrication, and mechanical properties. Sheet, 0.03 inch thick, was produced and its tensile strength measured between 250° and 1,935° C. The large particle size of electrowon tungsten effectively precluded sintering to a density sufficient to allow hot working to sheet or bar. The powders were consolidated by die pressing to 70-percent density, sheathing in molybdenum, and high-energy-rate extruding to either round or sheet bar of 100-percent density. The material was then rolled conventionally to sheet. The mechanical properties of the sheet prepared from the electrowon powders compared favorably with those reported in the literature for sheet prepared from commercially produced hydrogen-reduced powder.

Jan 1, 1970

By Joseph L. Condon

Fifteen shots of three explosives with charge weights of 0.52, 1.1, 3.1, and 5.1 kilograms were fired in a pond to study the seismic effects of detonating explosives in water. Shock pressures and bubble periods were measured with pressure transducers in the water. Vibrations were measured on land in three orthogonal directions with particle velocity gages. Statistical tests indicated that a charge weight exponent of 0.43 best scaled the data. While shock pressures and bubble periods showed considerable differences in explosive performances, the amplitudes of ground vibrations showed less difference, and one prediction equation was therefore derived to estimate vibration amplitudes from all the explosives.

Jan 1, 1970

By H. R. Babitzke

As part of a continuing project to develop refractory metal alloys for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation strengthening techniques to improve the properties of columbium alloys. The purpose was to investigate the effects of hafnium, tungsten, and boron on the formability, strength, and oxidation resistance of columbium. The experiment was of factorial design with two replications which called for 72 ingots of 36 basic compositions, weighing 150 grams each. Hafnium, tungsten, and boron were evaluated at 3, 3, and 4 levels, respectively. Values of alloy content are all in atomic percent. The highest strength observed was 29,000 psi at 1,200° C for alloys Cb-15Hf (No. 3), Cb-7.5Hf-5W-2B (No. 14), and Cb-15Hf-5W-2B (No. 15). At 1,200° C, the ternary alloy Cb-15Hf-5W (No. 6) which has shown good properties in previous Bureau of Mines investigations was the most resistant to oxidation For boron additions, the alloys oxidized more readily with increasing amounts of this element. The fabricability of the alloys high in boron became increasingly difficult, resulting in an inadequate number of alloys required for a complete statistical analysis for all the tests. As a result of the decrease in ductility, an insufficient quantity of tensile samples were available for a proper analysis for the high-temperature strength data.

Jan 1, 1970

By K. Thirumalai

This study forms a part of Bureau of Mines continuing research on thermal fragmentation of rocks. The potential of internal heating techniques for rock fragmentation is discussed. A concept of rock fragmentation with rapid inter¬nal heating of a localized inner volume of rock is advanced The energy required for rock fragmentation is made available by creating a required vol¬ume of localized heating. The fragmentation of rock using the proposed method is analyzed and qualitatively compared with the results of experiments with Charcoal granite, Dresser basalt, and Sioux Quartzite. High frequency dielec¬tric heating below 100 MHz is used in the study as an example to examine the working of the concept. The selection of operating conditions for the experi¬mental heating is explained. Fragmentation of Charcoal granite and Dresser basalt test rock blocks is achieved for localized heating below 550° C. The heated volume required for fragmentation is observed to be less than 2 percent of the test block volume and the electrical energy consumption is in the order of 3.5 to 6 5 kwhr/m3 The method offers a possibility for in situ fragmenta¬tion of rocks, favorable for internal heating. The method is highly dependent on rock properties governing internal heat generation The efficiency of dielectric heating in the experimental study is observed to increase with increasing dielectric loss of the rock material, ranging from about 10 percent in Sioux. Quartzite to about 50 percent in Dresses basalt

Jan 1, 1970

By L. A. Neumeier

The Bureau of Mines evaluated the properties of zinc alloys containing 25 to 40 wt pet Al and 0 to 0.7 pet Mg. Microstructures, hardness, and tensile properties were evaluated for material as extruded at 285° C, solution treated at 300° to 400° C, and subsequently aged at 100° to 200° C. The alloys without magnesium are characterized by low hardness and strength with high tensile elongation and reduction in area. It was verified that magnesium effectively retards the Zn-Al eutectoid transformation below 275° C and markedly increases hardness and strength with decreases in ductility. Solution treating at 350° C results in large grain sizes and gross embrittlement. Subsequent aging of the Zn-Al-Mg alloys at 200° C restores ductility substantially and stabilizes the structures, but strengths are considerably reduced. Combined strength and ductility properties are better for the as-extruded condition than for any heat-treated condition. There is usually little advantage in overall tensile properties from increasing magnesium above 0.1 pct.

Jan 1, 1971

By Galen G. Waddell

This report describes a method of measuring and analyzing the initial deformation which occurs in the medium surrounding a mine accessway as the opening is created. Discussed are (1) the hypothesis upon which the research is based; (2) the in situ rock-deformation measuring equipment developed; (3) the field tests, consisting of measuring the deformation of the medium around two 4-foot-diameter raise bores as the boring progressed; and (4) a finite-element technique to correlate theoretical with experimental results, using elastic theory. Described also are the raise-bore operation and performance. The instrumentation developed proved to have the sensitivity and resolution necessary to measure rock deformation around a full-scale raise bore during excavation. Tests show the relationships of rock deformation to progress of the raise boring and to time. The initial deformation of the opening appeared to be elastic. Using the deformation records and an estimated field stress, the modulus of elasticity was determined for the rock mass. In addition, the importance of this type of measurement in assessing support-problem areas is discussed.

Jan 1, 1971

By F. D. Sutterfield

This study was conducted to provide experimental evidence on the effect of modifications of gasoline front-end composition on the photochemical specific reactivities of automotive emissions. Evaporative and evaporative-plus-exhaust emissions from an automobile operated with four fuels of different volatility and varying levels of C.-C5 olefins were irradiated in a 10040 environmental chamber at three sets of initial hydrocarbon-nitrogen oxides concentrations. Reactivity was measured and expressed in terms of rate-of-NO2 formation and dosages of oxidant, peroxyacetyl nitrate, and formaldehyde. The compositional changes that were necessary in reducing fuel volatility were found to have no significant effect on the reactivity of the emissions. However, replacing C4-C5 olefins with saturated components resulted in sharp decreases in all reactivity manifestations observed for the evaporative emission samples. A lesser influence (of C4-C5 olefin replacement) was found with the composite exhaust-plus-evaporative samples; the effect that was observed could be attributed to the evaporative emission portion of the sample. The data therefore suggest that saturation of front-end fuel olefins had no large effect on exhaust emission reactivity.

Jan 1, 1971

By R. L. Rough

Photoelastic, wire resistance, and borehole-deformation gages were used to measure the in situ strains when an outcropping Black Hand Sandstone Formation in Hocking State Forest, Hocking County, Ohio, was overcored to stress-relieve the surrounding sandstone. Strains transmitted to the photo-elastic gage did not produce isochromatic patterns suitable for quantitative analysis. Strain readings from the wire resistance gage indicated tensile-strain loading during overcoring; readings from the strain-gage bridges in the borehole-deformation gage indicated compressive-strain relaxation during overcoring. The magnitude and orientation of the computed stress fields obtained from both gages were comparable when the corresponding tensile and compressive elastic moduli were applied. Stresses computed from deformation and resistance gages at depths to 5 feet showed the maximum stresses to range from 1.042 to 2.121 times greater than the minimum stresses. The bearings of principal stresses calculated from the deformation gage readings varied between N 61° E and N 83° E; the wire resistance strain gage bearing computations varied between N 68° E and N 82° E. Measurements of in situ strain in sandstone were shown to have promise but to require further development in field technique that could likely be achieved through experience.

Jan 1, 1971

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