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By R. E. Mussler

As part of an overall goal to develop technology that can maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines is evaluating a method for selectively extracting nickel and cobalt from low-grade domestic laterites. The method involves electrowinning to recover the metals in pure form; therefore, preliminary laboratory-scale electrowinning tests were conducted in both a nondiaphragm and a diaphragm cell to determine the effect of variables on energy efficiency under controlled conditions. Electrolytes were generally reagent-grade sulfate solutions that were prepared to simulate electrolyte that could be obtained by stripping nickel-and cobalt-rich solvent extraction reagents. Limited tests were conducted with electrolyte generated from laterite leach solutions. Electrical energy consumption in a nondiaphragm cell was 2.06 kwhr/lb Ni with the cell operated at 50° C, a cell feed of 90 g/l Ni, a pH of 3.5, an extraction of 3.2 g/l, and a cathode current density of 20 amp/ft2. The energy requirement decreased with increasing concentration and temperature, and increased with increasing. extraction and current density. At 50° C, energy consumption in the nondiaphragm cell was 21 pct greater than in the diaphragm cell, but it was only 5 pet greater at 65° C. For this reason and because of overall cost considerations, operation at 65° C with the nondiaphragm cell was preferred. Smooth sheets of cobalt were obtained by electrowinning in a nondiaphragm cell at selected temperatures from 50° to 85° C and with cobalt concentrations from 55 to 87 g/l. The energy consumption (1.48 kwhr/lb) was 22 pet lower with a cobalt concentration of 75 g/l and a cell temperature of 65° C than with a cobalt concentration of 55 g/l and a cell temperature of 50° C.

Jan 1, 1981

By T. O. Llewellyn

The Bureau of Mines, as part of its goal to develop technology that can conserve domestic mineral resources investigated beneficiation methods for recovering phosphate minerals from two Southern Florida deposits with high magnesium content. Chemical analyses of sized fractions indicated that no coarse pebble concentrate could be produced from either deposit. Conventional fatty acid-fuel oil batch flotation tests on two phosphate samples, analyzing 6.8 and 8.5 pct P205, yielded concentrates containing 28.97 to 29.80 pct P20S at recoveries ranging from 72.4 to 76.9 pct of the flotation feed. The MgO content ranged from 1.20 to 1.36 pct. Bubbling S02 gas through an aqueous concentrate slurry, further reduced the MgO content of these phosphate concentrates to 0.5 and 0.8 pct, but with a concomitant loss in the phosphate recovery. Settling characteristics of slimes from both phosphate samples showed a slow settling rate, which is a typical characteristic of other slimes in the region.

Jan 1, 1981

By William D. Riley

In order to evaluate the corrosion resistance of zirconium in mineral extraction processes, such as a clay-hydrochloric acid leaching process for extracting alumina, the Bureau of Mines conducted corrosion studies in HCl-AlC13-FeC13 environments. A series of weight loss and electrochemical tests were conducted at 25° and 65° C in aluminum chloride (AlC13) plus hydrochloric acid (HCl) solutions containing 0 to 1,000 ppm ferric ion. It was determined that zirconium, which normally exists in a passive state in chloride-containing solutions, undergoes pitting attack in solutions containing more than 100 ppm of ferric ion. It is also shown that an oxide film prepared in air at high temperature offers protection in acid solutions containing levels of ferric ion from 300 to 1,000 ppm.

Jan 1, 1981

By R. S. Olsen

The Bureau of Mines is engaged in a continuing research effort toward the recovery of alumina from kaolinitic clay and other nonbauxitic domestic minerals. Hydrochloric acid extraction of calcined clay is among the acid processes under consideration. Although aluminum is easily leached from calcined clay, the presence of fines and slimes in the leached residue has hindered the application of this and other acid leaching processes. A clay feed preparation method was therefore developed that eliminated the slimy nature and the separation problems normally associated with leached clay residues. The preparation process consists of crushing the raw clay to minus 20 mesh, dampening the crushed clay with a fine water mist while tumbling on a rotating disk, and calcining the misted clay at 750° C. The misting process increases residue settling rates threefold to 9 cm/min (18 ft/hr) and filtration rates by two orders of magnitude. Leaching-kinetics were determined for misted clay feeds in a batch, stirred-tank reactor. Rapid leaching occurred during the first 85 to 90 pct of the extraction. The linear relationship of extraction to time during this initial phase corresponded to a zero order reaction with a rate constant of around 10 pct/min.

Jan 1, 1981

By K. O. Bennington

The thermodynamic properties of synthetic acmite, NaFe3+Si206, were determined by the Bureau of Mines. The enthalpy of formation was determined by hydrofluoric acid solution calorimetry. The values of the standard enthalpy of formation at 298.15 K, ?Hf°298.15, from the elements and from the oxides, ?H°298.15, are ?Hf°298.15 = -615.87 ±0.71 kcal/mole, ?H°298.15 (from oxides) = -32.08 ±0.53 kcal/mole. Various experimental data were combined with other data from the literature to calculate all the related thermodynamic properties in the range of 298 to 1,263 K. The standard Gibbs energy of formation is ?Gf°298.15 = -575.8 kcal/mole.

Jan 1, 1981

By Bill M. Stewart

The Bureau of Mines conducted laboratory tests to determine the effects on the physical properties of coarse coal waste of adding large amounts of fine coal waste. Maximum laboratory dry density, optimum moisture content, shear strength, and permeability tests were conducted on samples that contained 18 to 60 pct minus No.4 (U.S. Standard sieve size) coal waste. For the nonslaky materials, maximum laboratory densities were highest and permeabilities lowest when the samples contained between 30 and 40 pct minus No.4. Shear strength increased rapidly when the proportion of minus No. 4 was increased from 20 to 40 pct, but then increased only slightly or leveled off when the minus No. 4 was increased to 60 pct. Optimum moisture content and permeability were the physical properties most affected by the addition of fines. Optimum moisture content increased as much as 3 pct, and permeabilities decreased up to three orders of magnitude. Slaky coal waste material had physical property reactions to the addition of fines substantially different from those of nonslaky material.

Jan 1, 1981

By E. D. Calvert

As part of its goal to minimize the requirements for critical and strategic minerals, the Bureau of Mines is conducting research to foster the use of domestically abundant materials such as molybdenum. This report describes the development of an investment shell molding technique that can be used to make castings of molybdenum and its alloys. The mold material is cubic Zr02 with a monoclinic Zr02 binder. The shell, formed by standard investment molding techniques described in the text, is prepared for molybdenum casting by firing for 6 hours at 1,550° C (2,822° F) or for 4 hours at 1,650° C (3,002° F). The resulting castings have predictable and reproducible dimensions with good detail. As-cast strength is poorer than the strength of wrought materials below 1,600° F. At and above this temperature, tensile strengths of cast and wrought materials are nearly equal. Aqueous corrosion of the castings in most media is insignificant.

Jan 1, 1982

By J. M. Kuchta

The Bureau of Mines investigated four simulated coal gob fires to obtain a more reliable data base for defining the state of a sealed mine fire and to evaluate the performance of various fire detectors. The fires were conducted in a multiple-entry section of the Bruceton Experimental Mine by heating 4,000 to 21,000 pounds of rubblized bituminous coal to ignition and monitoring the temperature, gas emissions, and smoke under ventilated and sealed combustion conditions. Product gas concentrations depended upon the coal bed size, coal temperature, heating rate, and oxygen concentration or ventilating condition but varied little after the fires were sealed. Expressions are given that define the temporal variation of CO and O2 after sealing when the coal temperature decreased rapidly. The CO/C02 ratio is a more sensitive fire indicator than the CO/?02 ratio, although the latter is universally used for detecting the incipient state of a coal fire. In comparison, the Jones-Trlckett ratio [ CO2 + ¾ CO ? ¼ H2 ?O2] is less reliable for this purpose. The best detector for determining the state of a mine fire after it has been sealed was a prototype submicrometer smoke particulate sensor. Limitations of the various detector systems are also discussed.

Jan 1, 1982

By Rolland L. Blake

Petrographic methods of examination were used by the Bureau of Mines on a suite of samples of ultramafic rock from Soapstone Ridge, Ga., located about 8 miles south-southeast of Atlanta. The samples were analyzed to determine (1) their potential for releasing regulatory particles upon crushing and grinding and (2) their concentration of fibrous particles that approach the dimensions of amphibole and serpentine asbestos minerals. Such particles might be generated during grading and excavation for housing and industrial development and could become a health concern. Light optical microscopy, scanning electron microscopy, and X-ray diffraction were the techniques used to examine the samples. Six of the twelve samples contained amphibole as a major mineral; in five, it was a moderate to minor mineral. One sample contained no amphiboles, and serpentine was not observed or identified by X-ray diffraction in any of the samples. In nine of the samples, the amphiboles exhibited a habit that was either prismatic or acicular, but not asbestiform. Two of the samples did contain asbestos, occurring as small veins or fracture fillings, which represented only a minor percentage of the total sample. Similar petrographic screening is recommended for examining any rock deposit or mine location to delineate hazardous and nonhazardous mineral areas.

Jan 1, 1982

This Bureau of Mines publication describes the plan used to instrument two longwall gateroads at the Powhatan No. 4 Mine of the Quarto Mining Co. Vibrating wire stressmeters, flat jack U-cells, multipoint extensometer stations, and convergence stations were installed in or on the coal pillars, roof bolts, and roof strata of the gateroad entries. The instruments measure pillar stresses, bolt loadings, and strata movements as the gateroad entries are developed and the longwall panel(s) is mined. The report details only the instrumentation plan of the longwall gateroads and not the evaluation of any subsequent data. This is because a complete analy-sis of the data cannot be made until extraction of the longwall panel(s) is complete.

Jan 1, 1982

By R. H. Lien

The Bureau of Mines developed a flue gas desulfurization process as part of its goal of minimizing the undesirable environmental impacts associated with energy and mineral-processing plants. The modified citrate process involves absorption of sulfur dioxide (S02) in a buffered citric acid solution. The S02-loaded solution is regenerated by countercurrent contact with steam in a packed tower. The wet S02 product is then dried and can be liquefied or further processed to make sulfuric acid. Test data from process investigation unit studies are presented. Material balances, flowsheets, and cost estimates are given for recovering S02 from copper smelter reverberatory gas, lead smelter sintering machine tail gas, and power-plant stack gas. Operating cost estimates show the process will add $0.04 per pound of copper, $0.01 per pound of lead, and $0.015 per kwhr to the cost of the respective operations. These costs could be substantially reduced if a source of waste heat was avail-able to provide the process steam requirements.

Jan 1, 1982

By David C. Oyler

Three long horizontal holes were drilled from a directionally drilled surface hole at the Emerald Mine near Waynesburg, Pa. The purpose was to adapt the technique of directional drilling for use in draining methane from coalbeds. A 504-m (1,652-ft) long, 76-mm (3-in) diameter, circular arc pilot hole was drilled, using a downhole mud motor, to enter the Pittsburgh coalbed at a vertical depth of 305 m (1,000 ft). The hole was reamed to 222 mm (8-3/4 in) and was cased to a measured depth of 486 m (1,595 ft). Three 76-mm (3-in) diameter horizontal drainage holes were then drilled, totaling 2,909 m (9,544 ft) of horizontal hole. Improvements in drilling methods increased the average drilling rate from 20.4 ill (67 ft) to 64.9 m (213 ft) per day. The cost of drilling the directional and horizontal holes (using a Government-owned drill rig) was $1,169,530, a figure inflated by inexperience and by delays caused by lost-circulation problems and fishing operations. An estimated total drilling cost of $960,000 (including rental of a drill rig) for an improved system, was determined by a detailed cost analysis. Initial gas and water production from November 1979 through May 1980 was low because of caving of the horizontal holes drilled in shale near the bottom of the casing.

Jan 1, 1982

By C. Melvin Lepper

Microseismic energy is generated when stresses accumulated in rock formations are released in the form of fracturing. The acoustic emissions resulting from these rock fractures and movements are detectable as velocity signals in the earth near the energy source. A Bureau of Mines microseismic system that is capable of detecting the acoustic emissions from pit slope movements is described. The digital circuitry incorporated in the system allows a microprocessor program to immediately calculate and present the location coordinates for the seismic energy source in the mine pit wall. This monitoring system is compact, portable, reliable, and relatively inexpensive and rapidly provides accurate information to the mine operators about the stability of a pit slope.

Jan 1, 1982

By Ernest W. Loya

A method for preparing gravimetric primary standards of helium in the parts per trillion range has been developed by the Bureau of Mines. The standards are used to calibrate a specially modified mass spectrometer used in determining the abundance of helium-3 and helium-4 in geochemical samples and of helium-3 in isotopically purified helium-4. The desired gas standards are prepared in 5-kg metal cylinders filled to 1,800 psia. Relative errors of less than 1 pct have been attained in the parts per trillion range using a successive dilution technique.

Jan 1, 1982

By W. L. Falke

The Bureau of Mines has developed a system that permits the "soft" soldering of aluminum and aluminum alloys with standard tin-lead solders. The method employs application of a thin nickel-copper-alloy coating to the substrate, which enables the tin-lead solders to wet readily and spread over the areas to be joined. With conventional technology, aluminum and aluminum alloys are extremely difficult to solder because tenacious surface oxide films prevent wetting. With the Bureau-developed method, the aluminum substrate is mechanically or chemically cleaned to facilitate bonding to a minute layer of zinc that is subsequently applied with an electroless zincate solution. The nickel-copper-alloy (30 to 70 pct Ni) coating is then applied electrolytically over the zinc, using immersion cell or brush-coating techniques. Development of acetate electrolytes has permitted deposition of the proper alloy coatings. The coated areas can then be readily joined with conventional tin-lead solders and fluxes. The joints so formed are ductile, strong, and relatively corrosion resistant, and exhibit strengths equivalent to those formed on copper and brass when the same solders and fluxes are used. The method has also been employed to soft-solder magnesium alloys.

Jan 1, 1983

By H. C. Ko

Heats of solution of calcium carbon-ate (calcite) and calcium oxide in hydrochloric acid were determined by solution calorimetry. Combination of these two heats yields a value of 42.643±0.024 kcal/mole for the enthalpy of calcination of calcite at 298.15 K. Literature data on ?H°298.15 of calcination of calcite were reviewed and compared. Thermodynamic properties for the calcination process were calculated from 298.15 to 1,500 K using Gibbs energy functions. This research was undertaken by the Bureau of Mines as an effort to provide thermodynamic data for the advancement of minerals technology, energy conservation, and environmental preservation.

Jan 1, 1982

By Michael T. Nigbor

The Bureau of Mines assisted the Rocky Mountain Energy Co. in a pilot-scale in situ leaching experiment at Casper, Wyo., to determine if sulfuric acid can be used as a cost-effective alternative lixiviant (leachant) for uranium in situ leaching. This experiment, which lasted more than 2 years, is the first fully documented pilot-scale operation in which the leaching-restoration cycle was completed using sulfuric acid instead of the more common carbonate-bicarbonate leachant This report describes activities at the experimental site, presents extensive geochemical data from startup to site restoration, compares laboratory and field experiments, and discusses the environmental aspects of acid leaching. The data showed that sulfuric acid is apparently an effective leaching solution. Three to five grams of acid per liter of ground water resulted in a production solution grade of 80 to 100 ppm uranium. Restoration was successful, but required extended flushing. The pH was the last chemical parameterto return to baseline, requiring about 350 days. This was longer than was predicted in laboratory simulations. The data also showed that mobilization of toxic elements such as selenium, arsenic, radium, thorium, and molybdenum stayed within reasonable limits and quickly fell back to preleach concentrations during restoration.

Jan 1, 1982

By L. J. Froisland

The Bureau of Mines conducted a 4-year research program at Uravan, Colo., on a 2-1/2-acre reclamation plot on the slope of a uranium tailings pile that had been covered with mine waste rock. The purpose of this study was to determine the effects of plant species, type of irrigation, type of fertilizers, and use of dust control chemicals on plant growth and surface coverage. Best grass coverage, nearly 100 percent with 240 plants per square foot, was developed in a section that was seeded with crested wheatgrass, fertilized with sewage sludge, and sprinkler irrigated. For comparison, a section that had been treated with commercial fertilizers developed 3.1 crested wheatgrass plants per square foot and 24 percent coverage without irrigation, and 8 plants per square foot and 75 percent coverage with irrigation. Results of spraying a dust control chemical were inconclusive. Russian-thistle invaded all test sections and ranged in density from 0.6 to 7.3 plants per square foot.

Jan 1, 1982

By J. S. Dunning

The Bureau of Mines investigated a series of Fe-Al-Mo alloys strengthened by ZrC (zirconium carbide) precipitates as chromium-free substitutes for stainless steels. Melting and fabrication methods were devised, and the effects of minor additions of columbium (niobium) and cerium on the mechanical properties and oxidation resistance were determined. Zirconium carbides could not be con-trolled reliably to produce fine precipitate dispersions. A more reliable carbide strengthening mechanism is required if the high-temperature strengths of types 304 and 316 stainless steels are to be duplicated. Workability and oxidation resistance of the alloy series were excellent.

Jan 1, 1982

By E. A. Johnson

The Bureau of Mines determined the effect of slag additives on copper solubility and the distribution of typical impurity elements between copper-iron matte and silica-saturated fayalite (iron silicate) slag at 1,250° C, in CO-C02 atmospheres with 10 pct S02. Small additions (<10 pct) of CaO, A1203, and MgO were shown to decrease copper solubility in the slag. Additions of CaO increased the solubility of bismuth and tellurium in the slag at lower matte grades. Al 20 3 additions decreased the solubility of tellurium in the slag, but increased that of bismuth at lower matte grades. A1203 additions increased the solubility of both at lower matte grades. With no additives, matte grade did not affect the solubility of bismuth in slags, whereas increasing matte grade resulted in a slight decrease in the tellurium solubility in slag. Additions of CaO or As203 alone to the slag increased selenium and arsenic distribution to the matte, but had little or no effect on antimony distribution; whereas small MgO additions decreased antimony distribution to the matte but had no effect on arsenic and selenium distribution. In slags with no additives, selenium distribution to the matte increased with increasing matte grade, while that of antimony decreased and that of arsenic was unchanged.

Jan 1, 1982