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By P. T. Brooks

Semipilot scale tests were made to demonstrate a newly developed electrorefining process which could be extrapolated to commercial scale in producing high-purity nickel and cobalt from crude nickel metal and high-grade ferronickel. The new process comprises application of solvent extraction techniques to remove and separate cobalt and iron from nickel and the electrodeposition in diaphragm cells of pure nickel and cobalt from chloride-based purified electrolyte. Using water insoluble organic amines, the solvent extraction operations enabled production of commercial-sized nickel and cobalt cathodes of higher purity than that of commercial electrolytic metals. The solvent extraction operation for separation of cobalt from nickel was made simpler than the conventional method. Furthermore, the solvent. extraction operation for iron removal made possible the electrorefining of ferronickel without the prohibitive loss of nickel resulting from the method ordinarily used for iron removal.

Jan 1, 1970

By Foster Fraas

Under a very high vacuum of 10-8 torr the transfer of terrestrial mineral beneficiation methods to the vacuum ambient of extraterrestrial locations such as the lunar surface was investigated. In the size range for the electro-static and magnetic separation of ores (minus 35 plus 150 mesh) there is no adhesion of particles produced by crushing and grinding due to the limited contact area, and for repeated contacts area size has a frequency of occurrence in accordance to the normal law. The photoelectric effect which is successful in separating a few minerals in an air ambient has a wider application in a vacuum, while the lack of air viscosity and sound transmission provides for high feed velocities and the adaptation of particle vibration to dispersion and grinding. Contact electrification is reversible upon return to atmosphere.

Jan 1, 1970

By C. M. Frost

The hydrodesulfurization characteristics of a residual fuel prepared from Wilmington, Calif., crude oil were determined at temperatures from 600° to 900° F, pressures of 200 to 800 pSig, and space velocities from 0.2 to 2.0 Vo/Vc/hr, using cobalt molybdate type catalysts. A prediction equation, developed from the experimental data, satisfactorily predicts the fraction of total sulfur that can be removed under any combination of operating conditions within the ranges investigated. Yields and properties of the low sulfur product are correlated with the fraction of total sulfur removed. Kinetic calculations show that the apparent reaction order and activation energy change with space velocity and temperature.

Jan 1, 1970

By Donald R. Johnson

Apparatus providing simultaneous differential thermal analysis, thermo-gravimetry, and evolved gas analysis, has been developed by the Bureau of Mines specifically for thermal study of oil shale and other solid, natural fuels. The apparatus is described in detail, and simultaneous analyses on a single sample of an oil shale mineral, nahcolite, and a thermal analysis demonstration compound, calcium oxalate monohydrate, are presented to demonstrate the instrument's capabilities.

Jan 1, 1970

By Frank G. Horino

This report presents a method of utilizing the Coulomb strength criteria for estimating the strength and stability of pillars and pit slopes containing planes of weakness. It is assumed that the Coulomb theory, as a special case of the Mohr envelope, is a satisfactory first approximation of failure in uniaxial compression or triaxial loading with low lateral loads. Accepting this assumption for brittle materials, an expression for the strength decrease of rock pillars containing a plane of weakness or fracture at any angle of orientation is derived. As few as six samples (three solid cores and three fractured cores at a failure-oriented angle) are required for testing uniaxially and triaxially to statistically determine the coefficients of friction and the shear strengths of both the solid rock and the fracture plane and the range of failure angles of the fracture plane. Interpretation of the data shows that the mean normal stress and maximum shear stress technique of analyzing the data is superior for solid core and that shear and normal stress values using angles of failure should be used for fractured specimens with failure-oriented angles. Plots of either the strength or strength ratios against fracture angles obtained from oriented drill core samples give a useful first approximation of strength decrease due to fracture. Using the same test conditions for both fractured and unfractured material increases the validity of the tests.

Jan 1, 1970

By Alfred E. Schwaneke

A versatile torsion creep tester was instrumented with electromechanical and servomechanical components to operate automatically and unattended, producing digital printed outputs. The apparatus uses an electrical system for applying torsional stresses, and a unique angular transducer as a null detector operating a servocontrolled strain measuring system with the digital readout. The tester is designed to measure the creep in single-crystal or polycrystalline zinc, zinc alloys, magnesium, magnesium alloys, or other metals and alloys. Applied stresses may be varied from zero up to 2,000 psi in the outermost fibers of a 1/8-inch-diameter, 4-inch-long specimen. Strain readings to 0.001 degree, equivalent to a strain of 2.73 X 10-7, may be made automatically from one every 5 seconds to one per month. The apparatus has provisions for programed temperature control and special atmospheres or vacuum operation. A discussion of applications of the system to other mechanical testing apparatus is included.

Jan 1, 1970

By John P. Hansen

Batches of red or brown iron ore concentrates, weighing 100 or 200 grams, were reduced with gaseous reductants in a laboratory-sized fluidized-bed reactor. Using a loss of weight technique, the rates of reduction were measured and the effects of temperature, gas consumption, and gas flow rates were determined. Below about 725° C the rate of reduction was controlled by the chemical reaction at the reduction interface having an activation energy of about 10 kcal/g mole. Above about 725° C the rate of reduction appeared to be controlled by the flow of the gaseous reductant and therefore to be directly proportional to the flow rate. Above 725° C, hydrogen reduced the iron ore much faster than carbon monoxide. In gas mixtures, carbon monoxide or nitrogen reduced the hydrogen partial pressure and lowered the reaction rate proportionally. When present in large concentrations, carbon monoxide had a serious inhibiting effect on the reduction rate, probably owing to carburization and sintering of the reduced iron.

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 E. G. Davis

This report summarizes an investigation to determine the occurrence and recoverability of heavy minerals in sand and gravel operations in the Southeastern United States. A total of 61 samples from 34 sand and gravel operations in Alabama, Georgia, South Carolina, and North Carolina were studied. Heavy minerals, in amounts ranging from 3 to 400 pounds per ton, were found in all of the samples. Eighty percent of the samples contained 20 to 40 pounds per ton of heavy min¬eral. Valuable heavy minerals, in order of decreasing amounts, were ilmenite, kyanite, zircon, rutile, and monazite. Large-scale concentration tests were made on five samples from four major producers. Gravity concentration by Humphreys spirals and tables resulted in bulk heavy mineral concentrates that graded from 82 to 98 percent total heavy minerals. Mineral recoveries ranged, in percent, as follows: Ilmenite 60 to 95; zircon 96 to 100; kyanite 37 to 77; rutile 89 to 100; and monazite 96 to 100. Separation studies on the gravity concentrates showed they would respond to high-tension and high-intensity magnetic separation techniques to produce individual mineral concentrates. The recovery of each individual mineral from fractionation of the heavy mineral gravity concentrates, in percent, was: Ilmenite 77 to 94; rutile 41 to 68; kyanite 62 to 79; zircon 49 to 83; and rare-earth products, monazite and xenotime, 42 to 96. The grade of each mineral concentrate was: Ilmenite 51.1 to 68.7 percent Ti02; rutile 93.7 to 94.3 percent Ti02; kyanite 55 percent A1203; zircon 58 to 61 percent Zr02; and rare-earth products containing 73.8 to 90.8 percent monazite and 4.8 to 12.7 percent xenotime.

Jan 1, 1971

By Robert Blickensderfer

Tungsten alloys with high-temperature strength properties, comparable to the best of alloys recently developed by others, were produced by a new process called here the oxyreaction process. The process involved additions of a powder of a reactive metal compound, ZrN, ZrW2, or HfW2, to a base metal powder, tungsten, which contained some oxygen. The powders were blended, compacted, sintered, and extruded. During sintering, diffusion and internal oxidation occurred to produce reactive-metal oxide particles and solid solutions. A dispersion of oxide particles could be precipitated by heat treating. The oxyreaction process circumvents many of the agglomerating and coarsening problems encountered in the current methods for dispersing a stable oxide in a metal. Oxyreaction strengthening results from solid-solution strengthening and from dispersion strengthening produced by the reactive metal and its oxides. At a test temperature of 1,650° C, the alloys prepared from WW, had tensile strengths up to 70,000 psi and stress-rupture lives up to 142 hr at 10,000 psi stress; the alloys prepared from ZrN powders had tensile strengths up to 80,000 psi and stress-rupture lives up to 27 hr at 10,000 psi stress. Tensile strengthening in the alloys was attributed to Zr in solid solution or to Zr-O-W structures too small to be observed in an electron microscope replica. Stress-rupture life was attributed to a dispersion of submicron Zr02 particles which precipitated and grew to 0.05-to 0.2-micron size during the test. Tensile strengthening and stress-rupture life were dependent upon both the zirconium and oxygen contents with the maximum occurring at roughly 0.9 atomic pot Zr and 0.9 atomic pot 0. Studies of the details of the oxyreaction process were made on the W-ZrW2 alloys and three general steps were determined: (1) The reaction of 0 in tungsten powder with ZrW2 to form relatively large Zr02 particles; (2) the dissolution of remaining ZrW2 into the W matrix and partial internal oxidation to form ultrafine but sparse zirconium oxide particles and possibly to establish Zr-O-W structures; (3) the development of ultrafine Zr02 particles during high-temperature aging.

Jan 1, 1971

By P. G. Pigott

This Bureau of Mines laboratory research demonstrated that building bricks meeting ASTM specification C62-66 for grades SW and MW of FBS-type bricks can be produced from waste copper mill tailings. Waste tailings from accumulations at Magna, Utah, Anaconda, Mont., and Hayden, Miami, and San Manuel, Ariz., were dry-pressed into bricks, and the products were tested in accordance with ASTM Designation C67-66 on sampling, and testing of brick. An evaluation derived from pilot-plant production of similar brick at the Coal Research Bureau of West Virginia University indicated the production cost to be about $34 per 1,000 bricks. Utilization of such mill tailings on a commercial scale would eliminate the need for digging new pits for brick raw material production, conserve natural resources, and simultaneously remove potential sources of air pollution.

Jan 1, 1971

By H. R. Appell

The Bureau of Mines is experimentally converting cellulose, the chief constituent of organic solid waste, to a low-sulfur oil, All types of cellulosic wastes, including urban refuse, agricultural wastes, sewage sludge, wood, lignin, and bovine manure, have been converted to oil by reaction with carbon monoxide and water at temperatures of 350° to 400° C and pressures near 4,000 psig, and in the presence of various catalysts and solvents, Cellulose conversions of 90 percent and better (corresponding to oil yields of 40 to 50 percent) have been obtained. A continuous reactor for use at maximum conditions up to 500° C and 5,000 psig has been operated successfully, Using sucrose as a feedstock, operation in this system has permitted a simplified and preliminary chemical study of the conversion process. Oil yields of over 30 percent have been obtained with this unit.

Jan 1, 1971

By R. A. Vik

The influence of thermal treatments on the grindability of low-grade hematitic iron ores from Michigan and Minnesota was examined in bench-scale tests. Treatment factors were roasting temperature, roasting atmosphere, and ore cooling conditions. Bond ball mill grindability and work indices were used as response indicators in evaluating the condition of the ore. Of the three treatment factors evaluated, roasting atmosphere, which brought about the con version of iron oxides to magnetite, had the most significant effect; roasting temperature had the next most important effect; and cooling condition had the least effect. Optimum grindability was obtained with reduced-quenched products of both ores at 650° C, near the alpha-beta phase transformation of quartz.

Jan 1, 1971

By M. M. Tilman

The Bureau of Mines conducted research into the dispersion strengthening of lead by the coprecipitation method. Commercially available reagents in water solutions were reacted to form homogeneous precipitates of lead and aluminum compounds. The resulting precipitates were roasted to oxides and reduced in hydrogen to form mixtures of lead powder and alumina. The powders were isostatically pressed into billets which were extruded into rods. The rods were rolled into strip to provide material for testing. Alloys containing 0.5, 1, 2, and 3 nominal volume-percent A1203 were tested in short-time tensile tests and in tensile creep tests. An alloy of Pb-3 volume-percent A1203 exhibited an average tensile strength of 8,570 psi after rolling to 75-percent reduction at 125° C but had no measurable elongation. Alloys of lower A1203 content provided a better compromise between tensile strength and ductility. For example, an alloy of Pb-0.5 volume-percent A1203 had an average tensile strength of 6,590 psi with 9-percent elongation after rolling to 75-percent reduction at 125° C. Creep rates of dispersion-strengthened Pb-A1203 alloys were below 1 percent in 10,000 hours at stresses of 2,000 to 4,000 psi.

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 William G. Pariseau

A small displacement-small strain finite element technique utilizing the constant strain triangle and incremental constitutive equations for elastic-plastic media that are nonhardening and obey a Coulomb yield condition has been applied to the analysis of gravity flow initiation in a V-shaped hopper containing a powder under lunar environmental conditions. Three methods of loading were examined. Of the three, the method of computing the initial state of stress in a filled hopper prior to drawdown by adding material to the hopper layer-by-layer is superior (as expected). Results of the analysis of a typical hopper problem show that the initial state of stress, the elastic moduli, and the strength parameters have an important influence on material response subsequent to the opening of the hopper outlet.

Jan 1, 1971

By D. W. Mitchell

This Bureau of Mines report summarizes experience and past research on methods for sealing abandoned areas of a coal mine and areas from which the pillars have been wholly or partially extracted. The Federal Coal Mine Health and Safety Act of 1969 requires that such areas be ventilated or sealed with explosion-proof bulkheads, but the present study indicates that bulkheads alone cannot isolate areas in a coal mine in which methane and other dangerous gases have accumulated. Gas-air exchanges between sealed and open areas must be controlled.

Jan 1, 1971

By A. W. Deurbrouck

This report describes the washability characteristics of 18 coal samples taken from 11 drill hole cores from the San Juan Basin area of New Mexico and Colorado. The ash content of these coals could generally be substantially reduced by removing the heavy impurities. The coals were characteristically low in sulfur content; only one sample contained more than 1 percent sulfur after removing the sink-I.50 specific gravity material. The coals ranged in rank from subbituminous C to high volatile C; 11 of the samples were subbituminous A. Many of these core samples came from areas where very little fieldwork has been done; consequently, an outgrowth of this work has been an increase in known coal reserves of the San Juan Basin area.

Jan 1, 1972

By Hillary W. St. Clair

This report gives the results of an experimental study of the progressive changes that occur in particle size and size distribution when a homogeneous and isotropic mineral is subjected to crushing by impact. The mineral used in the study was uniformly sized quartz, which was crushed in a simple drop¬-weight machine that applied impact energy up to about 100 kg-cm per g. Screen analyses of the crushed products were analyzed by the method of moments to determine the mean size, variance, skewness, and kurtosis. Analysis of the data from these experiments shows that the mean size of the crushed product is a function of the energy input and the initial size. The size distribution is functionally related to the degree of size reduction. As the mean particle size is decreased, at first there is a corresponding increase in the variance and decrease in the skewness, But, as size reduction is carried further, each tends eventually to approach a steady value, and the form of the size distribution becomes stable.

Jan 1, 1972