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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 B. J. Scheiner

As part of its mission to reduce pollution associated with mineral production, the Bureau of Mines is developing a dewatering technique for phosphatic clay waste that uses a flocculant, polyethylene oxide (PEO). This flocculant forms strong, stable flocs, which can be partially dewatered on a static screen and dewatered further on a rotary screen. Using this technique, a field test unit (FTU) was operated at a nominal 100 gal/min. Consolidated phosphatic clay material containing 20 percent solids was produced when feed slurries of 3 percent solids were treated with 0.69 pound of PEO per ton of feed solids. Pit and column tests indicated that the PEO-treated material continued to dewater; compacted products containing 40 percent solids were obtained after 45 days.

Jan 1, 1981

By G. E. McClelland

As part of its mission to assure an adequate domestic supply of metals essential to the Nation's welfare, the U.S. Department of the Interior, Bureau of Mines, investigated a particle agglomeration technique as a means for improving the flow of leaching solution through heaps of clayey or finely crushed, low-grade, gold-silver ores. Bench-and pilot-scale experiments showed that the percolation rate of cyanide leaching solution was markedly enhanced by mixing the ore with a portland cement binder, moistening the mixture, and mechanically agglomerating and aging the feed prior to heap building and leaching. The rate of gold and silver recovery markedly increased because of the increased, uniform percolation of leaching solution through the agglomerated feed. The use of concentrated cyanide solution instead of water during the agglomeration procedure decreased the leaching time required to obtain maximum recovery. Results of bench-and pilot-scale experiments are discussed.

Jan 1, 1981

By Karl R. Becker

Detonators representing a sampling of various domestic commercial delay detonators were fired at various direct-current (dc) firing levels. Results of firings using well-below-recommended firing levels showed marked increases in delay times above the nominal values. There was also a marked increase in variation, to the extent that out-of-sequence firings would be essentially assured in any typical blasting round at these low firing levels. Within the range of recommended levels the effects of current increases were not considered to be of great importance relative to other overriding effects, such as the significant difference noted in average values of detonators from different lots having the same nominal delay. This effect, when combined with the normal variation noted among members from the same lot, would cause out-of-sequence firings with detonators from a neighboring delay period. Where comparisons with results from another study were possible, it was found that both studies observed quite similar variations in delay times about the average values, and a lower probability of out-of-sequence firings for the shorter delay period groups. The criterion of the previous study for assessing the likelihood of observing out-of-sequence firings, when applied to the Bureau of Mines data, properly identified two neighboring delay period groups where out-of-sequence firings would occur.

Jan 1, 1981

By Jon C. Volkwein

The industrial sand industry has been exploring new techniques to reduce dust. One company was experimenting with adding water during bagging operations to the surface of the hag, and into the product as it flowed into the bag. The Bureau of Mines, using instantaneous dust sampling instruments, measured the effectiveness of three methods of adding water. Results indicated that various types of water sprays applied in carefully controlled amounts could reduce dust up to 50% at worker locations at the bagging machine and inside a railroad boxcar. This report also discusses constraints such as product handling, customer acceptance, cold weather problems, dust collector performance, and other areas.

Jan 1, 1981

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