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By S. E. Khalafalla

The Bureau of Mines investigated the metallothermic reduction of copper oxide as a function of temperature, reactant proportions, form of reductant, and gaseous environment, using iron and steel scrap reductants. The reaction proceeded rapidly with powdered iron at temperatures above 560° C, attaining over 95 percent copper metallization within 3 hours. The importance of inter-reactant contacts on the extent of the reaction was evident from the variable, but usually lesser, degree of metallization obtained with iron from tin cans and automobile steel scrap. Reduction decreased as the molar ratio of copper to iron increased between 1 and 3. The most favorable gaseous environment for the reaction was a static helium atmosphere containing about 0.6 percent water vapor. Ferrothermic extraction of copper from its oxides appears to be essentially a "solid-state cementation" process. While ordinary cementation processes must be preceded by leaching, the ferrothermic method avoids this generally slow step and also the water pollution caused by the leaching agents. Sulfidic copper concentrates could likewise be reduced with metallic iron following their complete oxidative roasting.

Jan 1, 1969

By D. E. Wolfson

Destructive distillation (carbonization) was shown to be a feasible method of disposing of scrap tires. The Bureau of Mines conducted tests under a variety of conditions. Solid, liquid, and gaseous products were produced, recovered, and analyzed. The quantities of the various products were shown to be quite dependent on the test temperature. Variability in composition of the liquid and gaseous products with changes in test temperature was also significant.

Jan 1, 1969

By J. R. Ruark

This report presents results of mining operations and of research and development work done during stage I of the gas combustion retorting research program conducted by the Colorado School of Mines Research Foundation and six major oil companies at the Bureau of Mines Anvil Points Oil Shale Facilities. A brief description of the gas combustion process is given and the experimental program is discussed. Included in this discussion are (1) air-gas distributor development, (2) results of gas and shale distribution studies, and (3) effects of other process variable studies. The report concludes with a statistical evaluation of experimental results. Two appendixes present a chronological account of the experimental work and tabulations of data for all retorting runs conducted during stage I.

Jan 1, 1969

By M. L. Whisman

Radiotracer techniques were developed for stoichiometric studies of photochemical reactions associated with atmospheric smog formation. Stock blends of separate hydrocarbon and oxygenated compounds were prepared and calibrated. 14C-labeled reactants and products in reaction systems involving hydrocarbons and nitrogen oxides at the ppm level were analyzed for qualitative and quantitative data. Precision and accuracy of these methods developed by the Bureau were determined by replication and statistical treatment of data, and these methods are described.

Jan 1, 1969

By Robert W. Ageton

The Bureau of Mines is currently conducting a comprehensive study to evaluate all aspects of recovering gold from large, low-grade deposits in the Golden Sunlight area, Whitehall mining district, Jefferson County, Mont. Prior to World War II this area produced significant quantities of gold. The study includes geologic mapping, diamond drilling, assaying, computer analysis of assay data, metallurgical research and ore testing, mine and mill planning, and an economic evaluation of all factors bearing on the establishment of a producing gold mine. Preliminary evaluation of the deposit indicates about 31 million tons of submarginal gold resources. American Exploration and Mining Co. (AMEX) has assisted the Bureau in this project by providing drill site preparation, control assays, and geological aid for the Bureau's exploration work and by furnishing comprehensive assay information of the property and copies of base and geologic maps. This report presents the geology and mining history of the area, together with a summary of Bureau work in progress.

Jan 1, 1969

By A. F. Colombo

Infrared spectroscopy employing attenuated total reflectance (ATR) techniques on thin films of dried gelatinized starch solution was used during Bureau of Mines research to determine the structural and impurity differences in starch products and to correlate these characteristics with the flotation response of a nonmagnetic taconite. All of the starch products evaluated gave spectrograms which were characteristic of the anhydroglucose monomer and its polymerization product. Distinct infrared absorption peaks caused by the protein molecule were observed and were used to classify the starches. Correlation of laboratory flotation of calcium-activated gangue from a Mesabi Range nonmagnetic taconite and infrared spectra produced from gelatinized starches showed that protein impurities and linear chain structure limited the effectiveness of starches as iron mineral depressants. Starch products having spectrograms similar to pure amylopectin were generally good depressants for iron oxides, were effective at about one-half the addition that was required for starches that gave infrared responses similar to pure amylose, and yielded acceptable iron concentrates containing 61.5 percent iron and 6.5 percent silica.

Jan 1, 1969

By L. C. George

The Bureau of Mines measured the vapor pressures of selected mixtures in the binary systems CdCl2 ?SnCl2, CdCl2 -ZnC12, PbCl2 ?SnCl2, and PbCl2 -ZnCl2 by the static pressure method. These data were evaluated by the second-law (sigma-plot) method. Equations expressing the vapor pressures and the heats and free energies of vaporization as functions of temperature are given.

Jan 1, 1969

By E. Morrice

Gadolinium, dysprosium, and yttrium are difficult to electrowin as high-purity liquid metals because of their high melting points (>1,300° C). Samarium metal is difficult to prepare directly by electrolysis because the metal reacts with the electrolyte. In this Bureau of Mines study, the rare-earth metal was electrodeposited on a solid manganese, chromium, or iron cathode to form a low-melting alloy. The alloy was then vacuum distilled to separate the rare-earth metal from the ferrous metal. A typical samarium metal product, obtained as the distillate from vacuum distillation of a samarium-iron alloy, contained 150 ppm oxygen, 80 ppm carbon, and 50 ppm iron as impurities, Gadolinium metal, obtained as a residue from the distillation of a gadolinium-chromium alloy, contained 300 ppm oxygen, 200 ppm carbon, and 100 ppm chromium.

Jan 1, 1969

By Hillary W. St. Clair

This report describes a mathematical procedure for analyzing size distribution data by the method of moments. The method was applied to Andreasen's data on a variety of grinding mill products. It was found that the observed size distributions could be represented by gamma and beta distribution functions over a wide range of sizes. A computer program, written in BASIC, is described for calculating moments, distribution parameters, and the weight fraction in any size range.

Jan 1, 1969

By H. W. Lang

The Bureau of Mines conducted an investigation to observe the effect of cetane improvers upon nitrogen oxides concentration in diesel exhaust gas. Amyl nitrite and amyl nitrate were used as additives to the fuel used in a four-cycle, single cylinder type test engine. It was concluded that nitrogen oxide concentrations were not enhanced at fuel-air ratios above 0.03 pound of fuel per pound of air.

Jan 1, 1969

By Richard E. Dawes

Physical variables, a principal factor in the economies of mineral production, affect both capital and direct operating costs. By using a revenue-cost system for the framework, the analyses of revenue and cost categories demonstrate the relative importance of groups of physical variables, whether explicitly defined or not, to a lead-zinc mining operation. Physical variables affecting the producer represent about 60 percent of the total system influence as expressed by cost ranking. Other physical variables affect the remaining costs as controlled by the smelter, the transporter, and the landowner. Such resource conservation aspects as mineral losses due to mining method and mineral processing constitute a portion of the total revenue effects of physical variables. The physical variable revenue-cost system presented in this report offers a framework for cost-benefit analysis of mineral related research.

Jan 1, 1969

By B. J. Dalton

The Bureau of Mines Helium Research Center has as a long-range objective the development of an equation of state for helium that will allow all of the thermodynamic properties to be calculated within the accuracy with which they are known. If this objective is to be realized, a method of calculation must be known. This report gives the principles of the method we use in such problems. A computer program was developed for predicting these properties, including those at the critical point, that is perfectly general and applicable to any equation of state. To demonstrate the efficacy of our method, this computer program was used to evaluate thermodynamic properties of a Redlich-Kwong fluid in the two-phase region. Expressions for calculating various thermodynamic functions specific for this particular equation of state are derived. Numerical values are tabulated and graphs are presented for all functions calculated. It is shown that for a Redlich-Kwong fluid there are finite discontinuities in (1) the second temperature derivative of the Gibbs free energy or chemical potential at the critical point, (2) the second derivative of the vapor pressure curve with regard to the temperature on passing through the critical point, and (3) the measured heat capacity at constant volume on passing through the critical temperature when the calorimeter is filled to the critical density. It is also shown that the heat of vaporization is infinite for a Redlich-Kwong fluid at absolute zero.

Jan 1, 1969

By D. H. Chambers

The Bureau of Mines developed a process for producing high-purity zinc and tin by electrorefining from liquid amalgams. Commercial grade metals were dissolved in mercury to produce saturated amalgams at room temperature. Amalgams were also prepared by electrolytic transfer from soluble anodes of the metals to a mercury cathode. Amalgams formed by both methods were used as anodes in electrorefining cells to produce high-purity cathodes. Metal impurities, excluding mercury, were at levels of less than 5 ppm in zinc and 9 ppm in tin. Mercury content was about 2 to 10 ppm in zinc products, and this was effectively removed by heating the cathodes in a vacuum. Mercury was excluded from tin cathodes by pumping the tin electrolyte through tin turnings and controlling the cell temperature.

Jan 1, 1969

By H. D. Jacobs

The Bureau of Mines developed a concentration method to upgrade and utilize marginal natural or direct-shipping iron ores and fine-grained lean iron ores. Presently these ores receive little beneficiation and accordingly have low iron-silica (Fe-Si02) ratios. Ore samples were roasted with equal weights of solid reductant at 1,100° C for 1 hour to metallize the iron and for an additional hour at 1,200° C to promote grain growth. Concentration was effected by crushing and screening techniques and/or wet magnetic separation. Sized concentrates (minus 4 plus 35 mesh) derived from crushing-screening processes contained from 80 to 85 percent iron that was 90 percent metallized. Iron-silica ratios as high as 12:1 and iron recoveries from 75 to 94 percent were obtained. The sized concentrates were judged suitable for use as blast furnace feed. Minus 200-mesh metallized concentrates derived from roasted minus I-inch plus 8-mesh ore fractions and magnetically concentrated contained 90 percent Fe and 4 percent or less Si02, chemically qualifying them as feed for electric furnaces. Roasting minus 8-mesh ore with hydrogen, then magnetically concentrating it, produced iron concentrates containing 57 percent to 67 percent Fe and 3.6 percent to 8.4 percent Si02. The concentrates having Fe-Si02 ratios ranging from 8:1 to 12:1 were considered adequate for use as blast furnace feed. Overall iron recoveries for the 12 ores tested ranged from 56 percent to 94 percent with an average iron recovery of 86 percent.

Jan 1, 1969

By D. Montagna

Large quantities of zinc-base die-cast scrap containing 3 to 4 percent aluminum are presently refined by mixing with other secondary zinc products such as galvanizer dross and distilling in a retort. The Bureau of Mines investigated alternate aluminum removal processes utilizing low-cost fluxes. Basing the investigation on the metallurgical principle that a reactive impurity can be removed from a less reactive matrix metal by melting under a flux consisting of a salt or oxide of a metal less reactive than the impurity, three separate flux mixtures were studied. In the first flux system, [FeCl3] + NaCI (the active component is underlined), part of the aluminum is' eliminated by the formation of volatile aluminum chloride and the rest by the creation of a high melting point iron-aluminum intermetallic compound that can be separated from the remaining molten zinc by filtration. Aluminum removal in the second system, [Fe203] + CaClz + NaCI, is effected by the formation of the iron-aluminum compound and possibly aluminum oxide. The third system, spent sal skimmings--essentially a mixture of [ZnCl2], NH4Cl, and ZnO, depends solely on aluminum chloride formation. Of the three flux systems investigated, the best results obtained were with system 3. Aluminum was reduced in the molten die-cast alloy from 4.10 percent to 0.01 percent when depleted sal skimmings were used.

Jan 1, 1969

By P. T. Brooks

This Bureau of Mines study describes a process for recovering nickel, cobalt, molybdenum, and chromium contained in complex waste superalloy grindings that, for lack of an economical domestic recovery process, are being largely marketed abroad. The process, devised by laboratory scale operations, includes scrap preparation, dissolution of metallics in hot chlorinated acidic liquor, carbon adsorption, three successive solvent extraction separations, and selective chemical precipitations. Nearly 90 percent of the nickel, cobalt, molybdenum, and chromium were separated and recovered as oxides, carbonates, and basic sulfate products.

Jan 1, 1969

By H. K. Kutter

The pressure pulse generated by an underwater spark \vas investigated in relation to its potential use for rock fragmentation. The study established (1) the relation between the peak discharge current and the peak wave pressure; (2) the relationships among the peak wave pressure, the discharge voltage, and the spark gap width; (3) the type and pulse duration of the generated wave; (4) the percentage of energy transmitted in the spark as a function of spark gap width and discharge voltage; and (5) the percentage of energy converted into the pressure wave as a function of gap width and discharge voltage. Spark-generated fractures were studied in two-and three-dimensional rock and plastic specimens. The laboratory results indicated that the pressure pulse generated by an underwater spark is a potential practical tool for rock fragmentation. The paper contains an appendix describing the capacitive pressure gage specially developed for the laboratory tests.

Jan 1, 1969

By C. M. Mason

A series of gelatinous permissible explosives was prepared with increasing sodium nitrate content and subjected to an improved technique for evaluating incendivity in coal dust-air and coal dust-gas-air mixtures. Those explosives containing an appreciable amount of sodium nitrate were found to be very hazardous in coal dust-air and coal dust-gas-air mixtures.

Jan 1, 1969

By W. H. Eddy

Laboratory batch and small-scale continuous flotation tests were con-ducted by the Bureau of Mines on a mica waste tailing from Kings Mountain, N.C., to determine the feasibility of producing high-quality mica, feldspar, and glass sand. Mica was recovered by two methods; one was by flotation in an alkaline circuit, which produced a mica concentrate assaying 92.0 percent mica with a recovery of 87.l percent, and the other by flotation in an acid circuit, which produced a mica concentrate assaying 91.0 percent mica with a recovery of 79.4 percent. Continuous flotation processing yielded a feldspar concentrate assaying 1.10 percent Na20 and 13.50 percent K20, with recoveries of 66.4 and 80.6 percent, respectively. The feldspar tailing was high-quality quartz glass sand analyzing 98.6 percent Si02 and 0.02 percent Fe203.

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