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By D. L. Pool

To increase metal recoveries and to minimize pollution by improved extraction technology, the Bureau of Mines investigated a hydrometallurgical technique to recover copper, lead, nickel, and cobalt from lead smelter mattes. The metals were converted from insoluble sulfides to soluble chlorides using a HCI-CI2-02 leaching system. Parameters studied in a 50-gallon, glass-lined reactor were the ratio of hydrochloric acid to chlorine, chlorine consumption per pound of matte, oxygen reaction pressure, and temperature. The matte material used contained, in percent, 19.7 Cu, 52 Pb, 2.9 Ni, 1.5 Fe, 0.38 Co, 0.19 As, 0.41 Zn, and 0.12 Cd. Extraction of Cu, Pb, Ni, Co, and Cd ranged from 92 to 98 pct, with concomitant extractions of Fe and As of <0.1 pct. The Cu and Pb were recovered as electrowon metals, while the Ni, Co, and Cd were recovered as mixed hydroxides.

Jan 1, 1981

By G. R. Palmer

Preliminary studies by the Bureau of Mines were conducted to determine the feasibility of a multiple-compartment, ion-exchange (MCIX) column simulator for examining the effect of multiple-orifice plates in the column. A rectangular, five-orifice, three-compartment, MCIX simulator with a cross-sectional plate area of 0.66 ft2 was used for the investigation. Orifices with open areas of 1, 3, and 5 percent were used with various operating conditions. The study was separated into three separate sections: (1) solution flow effect, (2) fluidization effect, and (3) resin transfer effect. The solution flow and fluidization studies showed that for solution flow rates of about 3 gpm/ft2, a I-percent open area plate functioned best, while at solution flow rates of 9 and 15 gpm/ft2, the best open areas were 3 and 5 percent, respectively.

Jan 1, 1981

By B. W. Madsen

As part of a program to maintain an adequate supply of minerals and metals to meet national economic and strategic needs, the Bureau of Mines conducted research to determine the diffusion coefficients for ferric ions in synthetic copper leach solutions. Determination of ferric ion diffusion coefficients in typical dump leach solutions is necessary for predicting leaching rates of copper from large-scale leaching operations and for optimizing concentrations of ferric iron in solutions to maximize leaching efficiency. Derivative chronopotentiometry, an electroanalytical technique, was used to determine ferric ion diffusion coefficients. The diffusion coefficient decreased dramatically with increasing concentration of iron in solution. An empirical model was used to relate the ferric ion diffusion coefficient to the total amount of sulfate in solution. Measuring the diffusion coefficient dependence on temperature yielded an activation energy of 5.5 kcal/mole of ferric ion. Activity coefficients of ferric ions as a function of concentration were calculated from diffusion coefficient data.

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 Jack C. White

The Bureau of Mines, in its efforts to insure the continued viability of the domestic minerals economy, has been engaged for several years in research on the extraction of alumina from domestic, nonbauxitic resources. Hydrochloric acid leaching of kaolin is one of the more promising technologies being studied for recovering alumina for feedstock to existing aluminum smelting capacity; 93 pct of this feedstock is currently imported either as bauxite or alumina. Organics contamination of pregnant leach liquor, originating during solvent extraction for removal of iron from aluminum chloride solution formed during hydrochloric acid leaching, causes rapid deterioration of the semihard rubber lining of process equipment. These organics were removed by a skimming tank-coalescer-activated carbon adsorption system. Organic levels of less than 10 ppm from the coalescer and less than 0.5 ppm from carbon adsorption were achieved. Analytical methods employing CC14 extraction and infrared spectrophotometry were developed to determine the organic content of both the liquor and the carbon. Mass transfer zones delineated in the carbon columns provide adsorption data for the design of larger systems.

Jan 1, 1981

By Noel N. Moebs

Studies by the Bureau of Mines have identified geologic structures in mine roof rock that contribute to many roof falls in Appalachian coal mines. These structures, including paleochannels, scours, pinchouts, slickensides, clay veins, crevasse splays, and joints, can often be identified during, and sometimes before, mine development. Mine projections can be revised to reduce the adverse effects of discontinuitites in roof structure; large roof areas of laminated sandstone or incompetent strata generally can be delineated or inferred from exploratory drill hole data, and the need for supplementary support can be anticipated. Accurate descriptions of roof geology also provide some indication of optimum length and type of roof bolts that should be installed.

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 V. R. Spironello

One of the primary objectives of the Bureau of Mines solid waste utilization program is the recycling of the magnetic fraction of municipal solid waste called raw refuse scrap. In this investigation, several types of scrap of differing quality, including refuse and turnings, were melted in a 1-ton electric-arc furnace in various combinations to produce steel in noncritical (construction) grades. In-formation on furnace operation and on the behavior of tramp and alloying elements was obtained. The research showed that it is possible to produce acceptable steel from a variety of steel scrap. Although some scrap is routinely used in steelmaking, it was found that up to 50 to 55 pct of the scrap charge can be ref-use, provided it is combined with higher quality scrap. The chemistry of the steels was generally acceptable, and all of them were rolled without difficulty. The specification (ASTM 615) for the steels produced was grade 40 or grade 60, containing 0.30 or 0.40 pct C, with mini-mum yield strengths of 40,000 or 60,000-psi, respectively. Most of the steels met the specification requirements. In-formation on typical microstructures of some of the steels is included. The composition of some furnace dusts showed high levels of Sn, Pb, and Zn.

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 T. G. Carnahan

The Bureau of Mines conducted research to simulate in situ leaching of a porphyry copper sulfide ore. The purpose was to determine the effects on copper leaching of additions of NaCI to a conventional sulfate leach system and to analyze the oxidant requirements and the oxidation products that resulted from leaching of the sulfide minerals in the ore. Baseline sulfate and sulfate plus 2-pct-NaCl-leach-solution experiments employing 167-kg (367-lb) and 152-kg (333-lb) charges, respectively, were conducted. The minus 25.4-cm (10-inch) ore was leached at 90° C under flooded conditions with 2.8 MPa (400 psig) of oxygen bubbling through the system. Sixty-seven pct of the copper was extracted in 1,236 days of leaching in the NaCI experiment, whereas 47 pct of the copper was extracted in 913 days of leaching in the baseline experiment. Diffusion into and out of the ore fragments controlled the rate of leaching, which precluded enhancement of the leach rate by the chloride ions. The calculated oxygen consumption was 3.17 kg/kg of copper extracted in the baseline experiment and 3.46 kg/kg of copper extracted in the experiment to determine the effect of chloride ions.

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 L. L. Oden

The Bureau of Mines analyzed vapor-aluminum-diffused stainless steels prior to conducting corrosion measurements in severely sulfidizing environments. These studies were conducted in response to the national need to better control the environmental and economic costs of corrosion. Specimens of a ferritic alloy and austenitic alloys types 316 and 310 were treated by a proprietary vapor-aluminum diffusion process and a dual vapor-aluminum diffusion process. Weights and dimensions were recorded before and after treatment, and comprehensive metallographic, X-ray, and electron micro-probe analyses were conducted for both single-and dual-vapor-aluminum-diffused specimens. Surface aluminum concentrations ranged from 26 to 34 wt-pct for all alloys. Dual treatment increased the quantity of aluminum per unit area by a factor of 2 and increased the depth of penetration by a factor of 3. The aluminum-diffused region of the ferritic alloy was single-phase aFe solid solution that was ordered on the surface, whereas two distinct diffusion layers were ob-served on the austenitic alloys. The outer layer comprised aFe solid solution that was ordered on the surface, and the inner layer was a two-phase mixture of aFe solid solution and the interrnetallic compound AINi.

Jan 1, 1982

By Sathit Tandanand

Geological differences among various coalfields restrain the applicability of subsidence prediction using empirical approaches previously developed. The Bureau of Mines assessed data collected from 16 longwall panels in the Northern Appalachian basin. Attention was focused on the effects of rock lithology, excavation width, and panel depth on the subsidence factor. The results show that the subsidence factor can be expressed in terms of the width-to-depth ratio by a simple exponential equation, which has a coefficient tentatively considered as the subsidence index. This index varies with the lithology of a particular site, and can be expressed in terms of percent distribution of weak and strong rocks in the overburden.

Jan 1, 1982

By G. B. Atkinson

Properties of catalysts prepared from intermetallic compound precursors were investigated by the Bureau of Mines as part of its mission to decrease U.S. dependence on foreign sources for scarce catalytic materials, such as nickel, cobalt, and chromium. Methods were developed whereby catalysts with surface areas of 30 to 40 m2/g were prepared from intermetallic compounds. Activity of these catalysts for the methanation reaction and methanol synthesis was deter-mined using a fixed-bed, single-pass, flow-through reactor. Catalysts prepared from rare-earth-nickel intermetallics had specific activity for methanation that was five times greater than that of commercial catalysts and were equal to or better than commercial catalysts with regard to sulfur tolerance. Under identical reaction conditions, catalysts prepared from thorium-copper intermetallics produced more than 10 times as much methanol as a commercial low-pressure catalyst and exhibited a high degree of catalytic stability.

Jan 1, 1982

By C. D. Litton

The results of full-scale fire tests are used to determine optimum distributions of fire sensors for the protection of conveyor belt haulageways in underground coal mines. Empirical relationships are derived that relate the spacing of fire sensors to the rate of development of the fire hazard. For this application, a critical fire size is defined as that size of fire for which belt ignition and subsequent flame spread down the belt is assured. Detection and alarm, regardless of sensor type or sensing methodology, must be achieved at some point in time before the critical fire size is reached. Based upon this approach, it is found that the horizontal spacing for products-of-combustion sensors is in the range of 300 to 600 meters, while the required thermal sensor spacing is found to be ~4 meters or less. Additional design criteria are discussed for product-of-combustion fire sensing systems.

Jan 1, 1982

By J. E. Pahlman

The Bureau of Mines conducted re-search to determine the resistance of basic refractories to corrosion by ash slags that would result from the burning of coal and lignite in metallurgical operations. Basic refractories are of economic interest because they are from one-third to one-half as expensive as 90-to 99-pct-alumina refractories. Static tests were performed at 1,300° C and dynamic tests at 1,400° to 1,650° C to investigate the stability of refractory specimens in a slag environment. In alkali-containing lignite ash slags, in order of decreasing resistance, magnesite, magnesite-chrome, and chrome-magnesite refractories all had corrosion resistances equal to or better than 90-to 99-pct-alumina refractories. These basic refractories formed slag penetration layers in dynamic tests, which helped protect them from further attack. Chemically bonded basic refractories in general did not have as good a resistance to slag attack as did burned refractories of the same composition. In very acidic coal ash slag, a chrome-magnesite refractory containing 30 pct MgO plus a slag inhibitor and direct-bonded magnesite-chrome refractories with 60 pct MgO had good resistance to attack. Chrome-magnesite refractories (30 to 40 pct MgO) were moderately to severely attacked, and refractories with greater than 70 pct MgO were severely attacked by this same slag.

Jan 1, 1982

By J. A. Eisele

As part of its goal of maintaining an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines has studied the removal of iron from simulated aluminum nitrate leach liquors by solvent extraction. Iron must be removed from aluminum nitrate liquor produced by leaching calcined kaolinitic clay with HN03 to reduce the iron level in alumina to less than 0.02 wt-pct Fe203 for use in reduction cells. The parameters reported are for (1) extracting iron from a feed containing 1.5 g/l Fe with di(2-ethylhexyl) phosphoric acid (EHPA), (2) stripping loaded organic phase with 20-pct HCI, and (3) water washing of loaded and stripped organic phase. Recommended operating conditions are two extraction stages using 15 vol-pct EHPA in kerosene and three stripping stages using 20-pct HCI. Results are also given for tests using other extractants and stripping agents.

Jan 1, 1982