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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

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 W. S. Sanner

A High Splint coal was carbonized in a low-temperature, fluidized-bed sys-tem to study the effects of thermal cracking on the products of decomposition. The coal was fluidized in recycle gas at 485° to 600° C, and the products were cracked at 600°, 700°, and 800° C in a bed of fluidized coke. Yields of tar, pitch, paraffins, and olefins decreased as carbonization temperature increased. Thermal cracking of the tar vapors produced the highest tar yields at 600° C, and light oil yield increased at cracking temperatures up to 700° C. At an 800° C cracking temperature, the yield of light oil decreased.

Jan 1, 1969

By E. G. King

Heats of formation of three crystalline oxides of rhenium (Re02, ReO3 and Re207) have been determined by the method of solution calorimetry, using an aqueous perchloric acid--ceric perchlorate solvent. Copper metal and cupric oxide were utilized as auxiliary substances. Heats were determined at 298' K for the reactions Re + 2CuO = Re02 + 2Cu, Re + 3CuO = ReO3 + 3Cu, and 2Re + 7CuO = Re207 + 7Cu. Standard heats of formation were derived using the value of -37.23 ±0,15 kcal/mole as the heat of formation of CuO. The standard molal heats of formation of the rhenium oxides were determined: Re02, -107.3 ±0.8 kcal; ReO3, -140.8 ±0.9 kcal; and Re207, -301.9 ±1.8 kcal.

Jan 1, 1969

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Beaver and Lawrence Counties, Pa. Washability analyses were made on seven coalbed samples, none of which were of metallurgical quality as received. Five of the samples could be sufficiently upgraded to produce acceptable products, and the remaining two samples could not be upgraded to metallurgical quality because their sulfur contents could not be lowered to meet the standard. For steam or power generation, one sample was of low sulfur content as received, one sample could be upgraded to low sulfur content, and three samples could be upgraded to medium sulfur content. The original sulfur content of the remaining two samples can be appreciably reduced by removal of the sink 1.58 speci fic gravity material; however, these coals would be classified as medium sulfur coals both before and after removal of the sink material.

Jan 1, 1969

By Marvin L. Whisman

A radiotracer technique developed by the Bureau of Mines extends to the parts-per-billion range the sensitivity for determining contributors of deposits formed in stored and thermally stressed jet fuels. The method depends upon measuring radioactivity associated with thermally induced deposits from fuels containing one labeled compound. The technique was applied to 88 test blends, representing 12 fuels and nine carbon-l4 labeled fuel constituents or fuel additives, or both. Data from results of these tests are included in this report. With this radiotracer technique, the contribution of fuel components and additives to thermally induced deposits in a variety of fuel environments was estimated before and after storage.

Jan 1, 1969

By A. Gene Collins

Some of the geochemical relationships that exist between subsurface fluids and the associated geologic strata in petroleum producing areas of Louisiana have been determined. Samples of petroleum-associated water were obtained from 126 wells in Louisiana that produced from sediments of three geologic ages: Tertiary, Cretaceous, and Jurassic. The samples were trans-ported to a central laboratory for analysis of chemical composition, using standard methods, to determine if the compositions varied with the geologic strata of their source and, if so, why. The dissolved constituents were com-pared with those of a brine that was concentrated by evaporation. The concentrations of bromide, calcium, and strontium were useful in distinguishing the brines produced from sediments of a late age from those of an earlier age. The concentration ratios of Mg' (total equivalent magnesium) and bromide indicated that dolomitization probably had occurred and altered the composition of the brines. A principal-components analysis of the data indicated an inverse relationship between depth and concentrations of bromide, strontium, calcium, and lithium.

Jan 1, 1970