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By Andrew J. Fergus

The purpose of this study was to provide basic information to aid further research on beryllium mineral flotation. Contact-angle and microflotation (Hallimond tube) methods were used to study collector action and flotation response of beryllium minerals and associated gangue minerals with representative commercial surfactants. Chrysoberyl received prime attention. Results indicated that selective flotation of beryl and chrysoberyl from fluorite and quartz is possible with sodium isooctyl phosphate below pH 2, and fluorite and topaz are readily collected by both anionic and cationic surfactants. Several modifying reagents were studied at one pH and one level of collector concentration. Aluminum sulfate, starch, and sodium silicate proved to be depressants in chrysoberyl flotation.

Jan 1, 1968

By James H. Aase

Selected glacial lake clay deposits in Minnesota were sampled, tested, and evaluated to determine their suitability for use as a bonding agent in iron ore pellet manufacturing. Preliminary tests conducted on clay samples obtained from five ancient glacial lake basins identified the clays in the Lake Agassiz glacial lake basin near Cook, Minn., as having the greatest bonding potential. An auger drilling program was conducted to obtain substantial quantities of representative material for detailed testing. The drilling indicated the presence of large clay reserves in excess of 500 million tons within the 12-square-mile area investigated. Bench scale tests indicated that the bonding properties of Cook area clays, when activated with relatively small quantities of sodium carbonate monohydrate (Na2C03?H2O), imparted excellent strength characteristics to iron ore pellets. Larger scale continuous pelletizing tests were made to confirm the bench scale results. These tests indicated that use of 1 percent activated clay alone as binder gave the iron ore pellets an overall strength slightly lower than with 0.75 percent bentonite, considered the industry standard. Use of 0.5 percent activated clay plus 0.5 percent bentonite produced better pellet strength qualities than use of 0.75 percent bentonite alone, without increasing the silica plus alumina content. The data from both bench scale and larger scale continuous tests suggest that the Cook, Minn., clays can be utilized after activation either alone or in combination with bentonite at an economic advantage over present pelletizing practice with bentonite.

Jan 1, 1968

By G. W. Weems

The Bureau of Mines used the Burnett method and apparatus to determine the compressibility factors for helium and carbon dioxide mixtures at 0°, 10°, 20°, 23°, and 35° C and to pressures of 900 psia. Tables of compressibility factors and approximations of the virial coefficients are presented for seven binary mixtures as well as for helium and carbon dioxide. The results compare favorably with existing data.

Jan 1, 1969

By Ronald P. Hollenbeck

Samples of clays, shales, and slates from 29 locations in the Appalachian Region of Alabama and Georgia were tested and evaluated to determine their suitability as raw material for the manufacture of lightweight aggregate by the rotary-kiln method. Samples from 11 locations in Alabama (one each in Etowah, Lawrence, and Morgan Counties and two each in Colbert, Cullman, Tuscaloosa, and Walker Counties) and one location in Walker County; Ga., produced satisfactory lightweight aggregate.

Jan 1, 1969

By R. K. Koch

The vapor pressures of liquid titanium and liquid platinum were studied under the Bureau of Mines program for the determination of thermochemical data on the transition elements. Beating was done in a 2-kw electron-beam furnace with a water-cooled copper crucible to contain the melt. Temperature was measured with a disappearing-filament brightness pyrometer. The vapor pressure data for liquid titanium in the range 2,008° to 2,379° K are represented by the least-squares derived equation [log p (atm) = 6.268 - 22, T] Two series of determinations were made on liquid platinum. Results of the first series are expressed by the least-squares derived equation [log p (atm) = 8.240 - 30,460T] for the range 2,0860 to 2,4200 K. Results of the second series are expressed by the least-squares derived equation [log p (atm) = 7.795 - 29,580 T] in the range 2,045° to 2,442° K. Third-law evaluations of each series gave mean standard heats of sublimation of 112.4 kcal/mole, 133.3 kcal/mole, and 133.8 kcal/mole for titanium first series on platinum, and second series on platinum, respectively. Second-law heats of sublimation and equations for heats, free energies, and entropies of vaporization were obtained from sigma plots of each data set.

Jan 1, 1969

By K-H. Frohne

This report presents a study of the Cooper sand of the Fork Run pool of Warren and McKean Counties, Pa., and a prediction of the secondary oil recovery by gasflooding the reservoir. A computer program employing a modification of the Craig, Geffen, and Morse secondary recovery calculation was used to make the gas flood performance forecast and is presented in the appendix. The Cooper sand reservoir in the Fork Run pool lies at a depth of about 1,900 feet and covers an area 1/2 mile wide by 2-1/4 miles long. Original oil in place is estimated to have been 8,266,000 STB. The primary recovery mechanism is solution gas drive, and ultimate primary recovery may reach 20 percent over a well life of 90 years. Two computer predictions were made for gas flooding the Cooper reservoir. The first was for a 25-acre pilot five-spot utilizing existing wells, but project economics were poor since only 25 percent of injection gas is utilized for pilot oil recovery. Recovery was 71,000 STB, or 22 percent of oil in place at flood initiation, but required 25,700 scf gas injected per STB of oil recovered. In the second prediction, pilot area performance was projected for the entire Fork Run pool, and economics became good. Recovery was 1,753,000 STB from 25 five-spots after the injection of only 6,400 scf per STB of oil recovered.

Jan 1, 1969

By Alton B. Cook

Data are presented to show oil vaporization resulting from the passage of natural gas through a sand-packed tube saturated with synthetic reservoir oils. The Bureau of Mines performed 13 experiments, using reservoir oils synthesized with base crude oils of approximately 22°, 35°, and 45° API, at 100°, 175°, or 250° F and 1,100, 2,600, or 4,100 psia. It has been determined that the amount of vaporization is significant if proper conditions exist. These experiments show that oil vaporization depends on pressure, temperature, volatility of the oil, and amount of gas cycled. Increases in each of these conditions increase the volume of oil vaporized.

Jan 1, 1969

By C. A. Komar

The Bureau of Mines conducted oil-displacement tests in the laboratory with three water-in-oil and five oil-in-water emulsions that were created with ultrasonic energy at a frequency of 20 kHz and an acoustic intensity of approximately 100 watts per cm2. Emulsions of either crude oil or kerosine, brine, and 112 to 2 percent emulsifier were formed during 30 seconds of acoustic irradiation. Results indicate that ultrasonic energy induces greater and more uniform dispersion of one liquid in another in the presence of small amounts of chemi¬cal emulsifiers. When the emulsions were injected as a buffer slug before waterflooding, recovery of the oil-in-place was 8 to 22 percent greater than with conventional waterflooding in the test specimens, regardless of the con¬tinuous phase (oil or brine). The emulsions do not appear to be applicable to the Appalachian area; however, because the oilfields are too "tight," the clays in the formation remove the emulsifier from the displacing fluid, and not enough additional oil is produced, compared with recovery using conventional waterflooding, to warrant the increased operating costs.

Jan 1, 1969

By R. S. Warfield

Several reconnaissance-type surface and drill core samples of Arctic Northwestern Alaska coals were taken during the summer field seasons of 1964 and 1966 for coking studies. Surface samples were taken from the Kokolik River and the Cape Beaufort areas; core samples were obtained from the Kukpowruk River and the Cape Beaufort areas. Only one Kokolik River surface sample possessed coking properties. This sample, representing an 11.6-ft coal seam, made coke approaching metallurgical quality when a 30-pct portion of selected blending coals was added. Four Kukpowruk River core samples, each representing the same 19-to 20-ft coal seam, were all of about the same coking quality. No differences of coke quality attributable to depth of permanently frozen overburden were found, but the data confirm previously reported information that the 19- to 20-ft coal bed is a potentially satisfactory base coking coal. In the Cape Beaufort area, a core sample with appreciable coking properties was taken at depth from a coalbed determined noncoking in a surface sample.

Jan 1, 1969

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 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 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 Richard L. Fischer

Constant-volume charges of precipitated PETN (pentaeythrite tetranitrate) at three specific gravities (0.50, 1.00, and 1.50) were used in laboratory tests to examine the effects of changes in explosive properties on free-surface displacement pulses and on crater dimensions. The tests were performed in large blocks of cement-mortar. The values for the detonation velocity, detonation pressure, specific energy, energy density, and energy release rate were calculated from the explosive loading density. Calculated explosive properties were correlated with free-surface displacement pulse measurements, strain energy, and measured crater dimensions. Increases in explosive properties resulted in increased free-surface displacement pulse parameters and crater dimensions. The loading density, detonation velocity, energy density, detonation pressure, and energy release rate were found to be best indicators of explosive performance. Simple acoustic relationships involving impedance ratios were examined and could not be used to predict peak displacement amplitude or strain energy. Data are presented in the customary English units as well as the International System of Units (SI).

Jan 1, 1970

By G. W. Weems

The specific objective of this investigation was to determine the compressibility factors for helium and carbon dioxide mixtures at -10° and -20° C and pressures to 1,000 psia. A Burnett apparatus was used. Data from the experiments were treated by the method of Barieau and Dalton. Tables of compressibility factors and approximations of the virial coefficients are presented for 10 binary mixtures as well as for helium and carbon dioxide. The results follow the same trend as data previously reported.

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 Harold A. Watson

A method for measuring leakage of vapors into a chemical-cartridge half-mask facepiece during simulated use is described. The respirator, fitted with high efficiency cartridges, is worn in a dichlorodifluoromethane (CC12F2)--air test mixture while a series of timed activities (facial movements, varied breathing, exercise, etc.) is performed. Complementing other tightness tests, this method is useful particularly for studying face fit and the effect of facial movements on leakage. The concentration of CC12F2 within the facepiece is monitored continuously to observe the immediate effect of physical activity on leakage. A composite sample is collected simultaneously in a plastic bag as a measure of average leakage during the 18-minute test period. Leakage, reported as percent, is calculated from the concentrations of CC12F2 within the facepiece and in the test atmosphere.

Jan 1, 1970

By Basil Dimitriades

The roles of hydrocarbons and nitrogen oxides in smog formation were investigated by the Bureau of Mines. Samples of automobile exhaust with varying HC and NOx levels were irradiated in a smog chamber under conditions that resulted in smog levels similar to those observed in the atmosphere. Results were used to define the patterns that describe the dependence of a number of smog manifestations on HC and on NOx. Using these dependence data and some simplifying assumptions, estimates were made of the ranges within which HC and NOx must lie in order to obtain specified levels of air quality.

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 Henry M. Harris

The roll forming of oxide powders was studied in a Bureau of Mines investigation to find the conditions and parameters required to make satisfactory ceramic strip. High-quality porous or dense alumina, zirconia, and porcelain shapes were made by sintering strip roll-formed at room temperature from powders containing minor amounts of binder and water. Strips with thicknesses of 0.04 to 0.08 inch and bulk densities from 40 to 90 percent of theoretical densities were made. The parameters most important to formability were particle size, condition of the powders, and roll gap. Other factors affecting quality were speed and surface condition of the rolls, amount and type of binder, water content, and sintering conditions. Ceramic strip was formed at rates up to 78 feet/minute, which is 13 to 23 times faster than reported by previous investigators, and forming was done in a simple and inexpensive roll unit. Reshaping the strip was possible by cutting, grinding, shearing, and stamping. The following innovations were developed that allow roll processing not normally possible with ceramic powders: (1) Fine-sized powders were made into strip by preparing these as partially sintered granules; (2) thick strip was formed by pressure feeding powders into the rolls; (3) flexible strip was made using a rubber-base bonding agent; (4) corrugated strip was formed on shaped rolls; and (5) porcelain strip was densified and reduced in thickness by rerolling while hot.

Jan 1, 1970

By P. T. Brooks

Mineral nodules from the ocean floor represent a vast potential source of manganese, nickel, cobalt, and copper. Process development studies to devise methods for recovering these metals were conducted by the Bureau of Mines using two types of nodules--relatively low-grade calcareous nodules from the Atlantic Ocean and higher grade siliceous nodules from the Pacific Ocean. Ammoniacal carbonate leaching of reduced nodules appeared to have the best potential for processing the calcareous nodules, but the method proved to be impractical for recovering manganese. Extraction of 90 percent or better of the nickel, cobalt, and copper showed the technique to be attractive for recovery of these metals. The siliceous nodules appeared amenable to a process that starts with either a sulfur dioxide leach or a sulfation roast followed by a water leach to dissolve the soluble sulfates.

Jan 1, 1971