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By John R. Hoskins

The Bureau of Mines conducted an investigation to more exactly define the influence of some end conditions on the laboratory-determined uniaxial compressive strength of rock samples. Limestone, marble, sandstone, and granite were used to provide a range of specimen modulus of elasticity from 2.7 X 106 psi to 10 x 106 psi. Four variables were studied: Nonparallelism and surface texture of specimen ends were the specimen variables investigated; the end platen size and the adjustable or spherical head friction were the machine variables studied. It was concluded that the loading ends of small laboratory models and samples should be prepared with surface irregularities that do not vary from a plane surface by more than 0.001 inch. It was also concluded that nonparallelism of the specimen ends should not exceed 8 minutes for a rigid head load or 15 minutes for an adjusting head load. The measured compressive strength of specimens prepared with these tolerances will be statistically the same with any diameter or thickness of platen and any degree of head friction if initial alinement of the specimen is assured.

Jan 1, 1968

By Elbridge W. Gresseth

Rock deformational structures in a deep mine were analyzed by petrofabric techniques to learn (1) the relative magnitude and direction of the principal stresses involved in tectonic deformations prior to mining, (2) the preferred orientation of rock planar discontinuities which define rock anistropy prior to mining, and (3) the relationship of mining-induced rock failure to inherent rock stresses and inherent rock anisotropy. Rock fabric elements used for petrofabric analysis consisted of bedding planes, faults, joints, fractures, foliation, sericite plane (001), quartz axis [0001], quartz deformation lamellae, and microfractures. Structures and structural symmetries from different areas within the mine and from different scales of observation were compared to learn the nature of rock anisotropy and the orientation of the principal stresses defined by rock deformations. Analysis of such fabric as regional and macroscopic faults, b-c joints, quartz [0001], sericite (001), and microfractures, indicate that during the epochs of tectonic deformation, the maximum and minimum principal stresses were horizontally oriented and acted along northwest and northeast axes, respectively. This condition of regional stress appears to have continued during folding and the associated period of faulting. The most recent tectonic deformation represents a rotation of the minimum principal stresses into a vertical position, as shown by the development of a tensile joint system, quartz deformation lamellae, and microfractures. Good interscale correlation and statistical homogeneity of tectonic fabric indicate a stress field homogeneity in this area during tectonic deformation. Rock physical anisotropy is genetically associated with tectonic fabric and consists of preferentially oriented planar discontinuities intersecting along a nearly vertical axis. The mining-induced deformations were correlated with the inherent rock anisotropy which either directly controls or greatly affects their development. This phase of rock deformation shows a greater degree of stress field heterogeneity than was the case with tectonic deformations This is explained as a result of nonconfinement afforded by underground openings and the increase in ground stresses due to mining activity"

Jan 1, 1968

By David E. Nicholson

The Bureau of Mines has constructed a special compression chamber for developing stress-strain relationships of mine backfill and simulating the high compressive ground pressures encountered in underground mines. A one-dimensional, or Earth-Pressure-at-Rest model is proposed for backfills subjected to these pressures. Results of the compression tests performed in the chamber indicate that reliable stress-strain relationships can be developed from these tests. The primary objective of the test series was to evaluate the effectiveness of compaction of common backfills in retarding ground closure. Analysis of the stress-strain data shows an eightfold reduction in relative strain in optimum well-graded, compacted backfills over poorly graded, loose backfill material. Analysis of the one-dimensional compression test data also indicates a significant retardation of transmitted stress in dense compacted samples of backfill and natural sands. Although not fully understood, a deformation mechanism is thought to occur at the intergranular contacts in cyclic fashion causing frictional heat loss and a reduction in transmitted stresses in the densely packed materials. The experimental values of transmitted stress are compared with theoretical values of effective stress calculated from the one-dimensional compression relationships developed by Hendron (4).3 These experimental values of transmitted stress compare very closely with the theoretical values of effective stress.

Jan 1, 1968

By R. H. Oitto

To determine whether reflectors could substitute for the trip lights referred to in the Federal Mine Safety Code, the Bureau of Mines studied trip safety devices under simulated haulageway conditions. The noticeability of reflectors compared with trip lights and fluorescent panels was evaluated from distances of up to 850 feet with light source intensities of up to 1-6 foot-candles (ft c). Reflectors tested consisted of a reflective lens in a holder secured to a frame that can be attached to a trip. Reflectors were found to be suitable for use as a trip safety device. In fact, for the conditions in many underground haulageways some reflectors would be more effective than a permissible trip light.

Jan 1, 1968

By M. E. Tyrrell

Research objectives were to determine the reasons for erratic behavior of semisilica horizontal zinc retorts in service; to investigate potential corrective measures including the possible utilization of more refractory materials in the retort body; and to delineate laboratory tests suitable for process control in the manufacture of retorts. Correlation of laboratory test results and data supplied by the cooperating smelters indicated that structural failures due to thermal shock and laminations in the retort body are largely responsible for the erratic behavior of horizontal zinc retorts in service. The most promising modifications made in the retort body and evaluated on a laboratory scale included finer grinding of the plastic clay fraction, substitution of mullite grog for calcined fire clay and grain alumina for silica, plus the use of an organic binder. Lamination-free extrusions having excellent thermal shock resistance were prepared from a mixture composed of 50 percent low-silica Missouri plastic clay through 100 mesh, 25 percent mullite grog through 6 mesh, and 25 percent alumina through 100 mesh. The mix was pugged under 28-inch vacuum with 1 percent ligno sulfonate binder in 12 percent tempering water. Laboratory tests suitable for process control in the manufacture of retorts are described.

Jan 1, 1969

By C. C. Merrill

The Bureau of Mines beneficiated the wastes generated by commercial titanium chlorination operations to reclaim metal values and reduce the problem of disposing of solid wastes. A water leach solubilized about 40 percent of the dry weight and over 75 percent of the metallic impurities. The residue from the water leach was rich in titanium dioxide and carbon; it was combined with rutile and recycled to a laboratory chlorinator. The contained carbon was used in lieu of part of the coke requirement.

Jan 1, 1969

By M. M. Fine

Research on the solid-fuel reduction of Knob Lake iron or was conducted to upgrade lean and high-grade ores and recover metallized products suitable for ironmaking or steelmaking. The program included bench-scale tests plus a number of continuous campaigns in a 34-inch by 36-foot rotary kiln. In the laboratory, metallizations in excess of 90 percent were achieved by reduction of crushed ore with lignite at 950° C. Subsequent grinding (to minus 200 mesh) and wet magnetic separation yielded concentrates analyzing less than 3.0 percent SiO2 and more than 90 percent Fe. Virtually complete recovery of the iron occurred. During early continuous tests the crushed ore created a serious ringing in the kiln which was solved by balling the fines with bentonite. Unfortunately, at this temperature (950° C) the bentonite militates against the concentratability of the metallized product. For example, a run on direct-shipping ore produced concentrates of 89.5 percent Fe and 4.5 percent SiO2. At 500° C the adverse effect of bentonite disappeared and concentrates of 88.4 Fe and only 2.5 percent SiO2 resulted. However, with comparable feed r Los, the metallization dropped to 73 percent.

Jan 1, 1969

By Donald C. Strimbeck

The Bureau of Mines designed a down-fired refractory-lined combustor that efficiently burned pulverized coal to produce a gas suitable as working fluid for an open-cycle gas turbine. The gas contained relatively little carbon, so the load on the ash-separation equipment was significantly reduced. Moreover, reduction in carbon content of the gas increased the average density of the solid particles making them more amenable to removal by centrifugation. Centrifugal-type separators failed to remove sufficient ash; however, to limit blade wear enough to achieve operating periods generally deemed necessary for commercial practicability.

Jan 1, 1969

By Jack L. Henry

The ternary system A14C3-AIN-Al203 has been examined to determine compositions which may display desirable high-temperature refractory properties. Powder methods were employed in the synthesis of all test compositions. Forming and sintering behavior was examined and hot-pressing parameters were measured. Several properties were studied for each composition of interest in the system. The properties included hydrolysis rate in moist air, elevated temperature oxidation rate, density, softening point, tensile strength, and rupture strength. In most cases equilibrium was not achieved, and the data are representative of a nonequilibrium system. Approximately 16 separate phases have been observed in the system. Forming behavior and selected properties of five compositions of interest were compared with those of aluminum oxide and aluminum nitride. None of the compositions compared favorably. Oxidation and vaporization appear to be serious drawbacks to the use of these compositions at elevated temperatures.

Jan 1, 1969

By D. A. Keefe, O&apos

The electrowinning of beryllium from beryllium oxide (BeO) using a molten-salt electrolyte composed of 56 LiF-37 BeF2-7 BeO (mole-percent) was investigated. Anodes made of porous carbon were found to be superior in current-carrying capacity and gave a lower cell voltage than other types of anode material tested. When porous carbon anodes were used) the resultant increase in anode area prevented anode passivation. The cell voltage was 3.3 volts) and electrode current efficiencies of 50 to 70 percent were obtained. The electrodeposited beryllium was recovered as beryllium powder or was coalesced to metal beads by heating to 1,300° C.

Jan 1, 1970

By D. E. Kirby

The electrochemical reduction of AlC13 was investigated as a process for the production of aluminum. An externally heated, single-compartment cell with a rammed refractory lining was used with molten KCl-NaCl-AlC13 electrolyte. Aluminum was deposited qt 700° to 760° C with a current of 100 to 200 amperes on a molten aluminum cathode. Chlorine was evolved at a graphite anode and collected and measured to provide a quantitative evaluation of the AlC13 reduction. Aluminum was removed from the cell by siphoning or ladling. Granular AlC13 was added periodically to replenish that depleted from the electrolyte. Concentrations of 7.5 to 17.5 percent AlC13 in the electrolyte were optimum for operation. Anode current efficiencies of 83 to 85 percent were attained, using anode current densities of 5.9 amperes per square inch and an anode-cathode distance of 4 inches. The chemically bonded, alumina liner was resistant to attack by aluminum and chlorine but susceptible to erosion at the surface of the electrolyte. Titanium diboride proved suitable for the electrical connection to the molten aluminum cathode. Aluminum of a purity equal to or better than 1100 series metal was electrowon continuously from commercial AlC13 for a period of 4-1/2 months.

Jan 1, 1970

By V. A. Cammarota

In this report, the effects of anode-production variables, such as aggregate coke sizes, pitch binder content, and baking cycle, were investigated. A small alumina reduction cell proved effective in evaluating anodes prepared from commercial materials and from lignite coke and pitch. Compressive strength was found to be the physical property most significantly influenced, but it did not appear to affect anode consumption. Specific carbon consumption, that is, the ratio of carbon in the anodic gas to carbon theoretically oxidized at the anode, was used as an index of anode consumption. It was found that an anode made with lignite coke and commercial pitch was very low in consumption; however, anodes made completely from lignite but by a different fabrication method showed high consumption and anode deterioration. Microscopic examination of anodes after electrolysis showed evidence of higher consumption at low current densities, and was useful in judging overall anode quality. Based on the physical properties of the anodes and their consumption during electrolysis, lignite can be a suitable material for anodes, provided the proper fabrication conditions are used.

Jan 1, 1970

By Larman J. Heath

Wellbore enlargement was tested using hydrazine hydrate in a gas-storage well in Ohio to increase the well productivity. The wellbore was to be enlarged by chemical disaggregation of the sandstone adjacent to the wellbore. Productivity immediately declined 49.1 percent and gradually declined to zero in 7 months. A down-hole camera survey showed a white-to-gray precipitate covering the entire wellbore surface. The precipitate was chemically analyzed and identified as mostly carbazic acid, a hydrazine derivative of carbonic acid. Formation of this precipitate was not anticipated; this viscous sub-stance caused the gradual loss in productivity of the well. The wellbore was not enlarged. Laboratory tests were run to determine what clay stabilization measures could be taken in sandstone cores to prevent clay swelling and particle migration caused by hydrazine hydrate. Normal clay stabilization methods did not prevent the virtually complete loss in permeability to hydrazine hydrate. Other laboratory tests using natural gas diluted with small amounts of carbon dioxide confirmed the ease with which carbazic acid could be formed in a hydrazine hydrate-saturated environment within and adjacent to the wellbore.

Jan 1, 1970

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