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By J. E. Matta

The Bureau of Mines has developed a tracer gas method for measuring leak-age through permanent mine stoppings. In this method, a temporary brattice is erected in the same entry as the leaking permanent stopping. Leakage was evaluated from concentration measurements of a tracer gas introduced into the space between the stopping and brattice. Stopping leakages ranging from 15 cfm to 265 cfm were simulated in an underground coal mine. Leakage values determined by the new method were within 10 pct of the known values.

Jan 1, 1978

By A. F. Colombo

In an effort to maintain an adequate supply of iron to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is conducting research on methods for beneficiating the oxidized taconite resources located on the western Mesabi range in Minnesota, thus expanding domestic iron ore reserves. The selective flocculation and cationic flotation process was investigated in a pilot plant using an ore feed rate of 410 kg/hr (900 1b/hr) and 88 percent recycled water. Lime and a cationic flocculant were used to clarify the waste slurries treated in the water reclamation circuit. An oxidized taconite assaying approximately 36 percent Fe yielded concentrates averaging 63.5 percent Fe and 4.3 percent SiO2 and having an average iron recovery of 84.4 percent. The estimated reagent cost per tonne of concentrate was approximately $1.10. In an attempt to recover more of the iron lost in the flotation tailing, wet high-intensity magnetic (WHIM) separation was incorporated in the pilot plant circuit. The flotation concentrate grades obtained from beneficiation circuits with and without WHIM scavenging were similar, but when WHIM separation was used the overall iron recovery was increased by 2 to 9.5 percent, depending on the iron assay of the flotation tailing.

Jan 1, 1978

By J. C. White

A research study was conducted to devise a method for producing phosphoric acid directly from unbeneficiated Florida phosphate matrix. This research was performed as part of the Bureau of Mines, U.S. Department of the Interior, goals of improving minerals and metals recovery from domestic resources and of minimizing the environmental impact associated with mineral recovery operations. This report describes research in which unbeneficiated, dry, south-central Florida phosphate matrix was digested with sulfuric acid in a continuous-circuit, five-tank reactor to yield phosphoric acid and gypsum residue. Feed capacity of the reactor was 100 pounds (45 kg) of dry matrix per 24-hour day. When digestion was carried out at 185° F (85° C), acid filtration rates of up to 420 pounds of P20S per square foot per day were attained. Combined iron and aluminum impurities in the product filter acid were about 60 percent greater than values reported in commercially produced acid derived from concentrate. phosphate recovery was 87 to 90 percent of the phosphate contained in the as-mined matrix.

Jan 1, 1978

By J. H. Heginbotham

As part of the total metallurgical system to recover metals from secondary resources, the Bureau of Mines conducted froth flotation research, using cationic reagents to recover glass from urban refuse. Batch flotation tests showed that high-quality cullet can be obtained from glass-rich aggregates derived from municipal incinerator residues and unburned refuse. This was confirmed by pilot plant operations treating 350 pounds of flotation feed per hour. Aggregates containing 85 to 90 percent glass were wet-ground to minus 20 mesh, deslimed in two stages, and fed to flotation cells. The glass was selectively floated using an amine collector, usually in an amount under 0.2 pound per ton of solids in the feed. The glass concentrates from the rougher cells were cleaned by refloating two or three times. Over 90 percent of the glass in the deslimed feed was recovered in the cleaned concentrates.

Jan 1, 1978

By D. E. Traut

The effect of various ion concentrations on uranium absorption from a sodium carbonate solution by a strong-base, anion resin was investigated by the Bureau of Mines in support of its objective to help assure an adequate uranium supply for future needs. The studies were conducted to improve the recovery of uranium from in situ leach solutions by ion exchange. The effects of carbonate, bicarbonate, chloride, and sulfate ions were examined. Relatively low (less than 5 g/l) concentrations of chloride, sulfate, and bicarbonate were found to be detrimental to the absorption of uranium. High (greater than 10 g/l) carbonate concentrations also adversely affected the uranium absorption. In addition, the effect of initial resin form was investigated in tests of the chloride, carbonate, and bicarbonate forms; resin form was shown to have no effect on the absorption of uranium.

Jan 1, 1979

By R. P. Beyer

Low-temperature heat capacities and standard enthalpy of formation of copper difluoride (CuF2) were determined by the Bureau of Mines. The low-temperature heat capacities were determined from 11 to 302 K by adiabatic calorimetry. The enthalpy of formation was determined by HC1 solution calorimetry. The standard values of entropy (S°) and enthalpy of formation (?Hf°) at 298.15 K are l8.65±0.03 cal/deg mole and -129.02±0.29 kcal/mole, respectively.

Jan 1, 1978

By E. F. Ferrell

The Bureau of Mines, U.S. Department of the Interior, studied the use of manganese sea nodules for catalytic oxidation in air of 1 pct carbon monoxide, 1 pct propane, and 1 pct methane. Catalysts were prepared from both Pacific Ocean and Atlantic Ocean nodules and compared with a platinum catalyst using a fixed-bed, steady-state microreactor with gas chromatographic analysis. Combustion temperatures with manganese nodules were 50° to 100° C lower than those with the platinum catalyst. Ion-exchange addition of rare-earth promotors to the nodule catalyst decreased combustion temperatures an additional 5° to 45° C.

Jan 1, 1978

By T. G. Carnahan

The Bureau of Mines investigated a flotation-nitric acid leach procedure as part of the goal to maximize minerals and metals recovered from primary and secondary domestic resources. Studies were conducted on an ore that contained carbon-bearing and sulfide mineralization that rendered a portion of the ore refractory (resistant) to conventional leaching technology. The procedure investigated for treating the ore consisted of the following: (1) separation by flotation of the carbonaceous and sulfidic components from the ore, (2) leaching the flotation concentrate with nitric acid at 100° to 110° C, (3) leaching the flotation tailings with sulfuric acid, and (4) processing the combined leached slurries in a conventional manner to recover yellow cake. In step 2, HN03 is converted to gaseous products from which it is regenerated by reacting these products with air and water for further leaching. An overall uranium extraction of 96 pct was achieved by this procedure.

Jan 1, 1979

By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By Edward F. Divers

This Bureau of Mines report describes the results of a laboratory evaluation of a mechanical dust collector (scrubber) suitable for underground coal mine applications. The scrubber was developed by the Mining Research and Development Establishment (MRDE), Burton-On-Trent, England, and tested at the Federal Bureau of Mines Pittsburgh Mining and Safety Research Center (PMSRC) as part of a technical exchange program. The 2,000-to 8,000-cfm scrubber consists of an electrically driven vane-axial fan, water sprays, a 2-inch-thick, loosely knit stainless steel wire filter panel, and a water droplet eliminator. The dust-laden airstream travels axially through the water sprays, filter panel, fan, and eliminator. Slurry water drains into a sump where a belt-driven pump recycles it back to the sprays. Fractional breakdown tests showed a maximum dust collection efficiency of 96 pct of respirable-size (less than 7 µm) coal dust at 2,000 cfm. Efficiency decreased with increasing airflow; for example, to 91 pct at 6,000 cfm. Following these tests the original wire panel was replaced with a similar but smaller panel developed at PMSRC; a marked improvement in dust collection occurred at all flow rates tested.

Jan 1, 1979

By J. E. Pahlman

One of the goals of the Bureau of Mines is to develop metallurgical pro-cesses that conserve energy and/or that take advantage of abundant domestic energy sources. Western lignites and subbituminous coals can be used for firing pellet induration and metallization furnaces. However, the refractory linings of these furnaces must be able to withstand attack from corrosive alkali metal oxides present in the ash of many of the low-rank fossil fuels. The Bureau of Mines conducted dynamic and static slag tests on high-alumina and alumina-silica refractories to determine their resistance to lignite ash slags. The investigations showed that increased alkali content in the lignite ash caused increased corrosion and erosion of the tested refractories. The degree of corrosion decreased with increasing alumina content, with the 99-percent-alumina refractories having the highest resistance. In general, the matrix phase was attacked preferentially to the alumina grains. Also, porosity reduction and tar impregnation enhanced the corrosion and erosion resistance. The 90-to 99-percent-alumina refractories are recommended for use as furnace linings in alkali slag environments.

Jan 1, 1979

By J. S. Hansen

In support of its objective to conserve mineral resources by minimizing premature failure of materials, the Bureau of Mines conducted a cooperative study with the U.S. Department of Energy on the erosion and abrasion resistance of hard materials for valves in coal conversion systems. This report describes a newly developed erosion-testing apparatus and presents data on the erosion resistance of over 200 materials. Erosion resistance of most metals was comparatively low. In contrast, ceramics and cermets such as B4C, WC, SiC, Si3N4, and TiB2, when fabricated to minimize porosity, displayed greater than five times the erosion resistance of metals. Coatings such as boron diffused into Mo and WC, chemical-vapor-deposited TiCN, and electrodeposited TiB2 were highly erosion resistant if applied in thicknesses ranging from 60 to 75 µm. Erosion resistance of cemented carbides was inversely related to metal binder content.

Jan 1, 1979

By Raymond F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Albany Metallurgy Research Center has developed atomic absorption spectrographic methods for the rapid analysis of A1203, CaO, Fe203, MgO, MnO, and Si02 in steelmaking slags. The application of these methods is discussed using an inexpensive pressure dissolution system. The overall coefficient of variation is 5 pct. The accuracy is the same as the reproducibility.

Jan 1, 1979

By A. Visnapuu

The Bureau of Mines, as a part of its goal to minimize occupational hazards associated with mining and mineral processing operations, has developed and field tested a compact exhaust air muffler for mechanized, jumbo-mounted pneumatic rock drills. The muffler is constructed of 1/8-inch sheet steel and has nominal dimensions of 1-3/4 by 9 by 13 inches. A directed air passage, flexible neoprene baffles, and an expandable slit-type outlet are incorporated to reduce drill exhaust air noise and eliminate muffler icing. Field tests in actual mining operations showed a l5-dbA reduction in exhaust noise and an 8-to 12-dbA reduction in overall drilling noise with no icing problems or decrease in drill performance. Data are presented on muffler construction, laboratory, and field test results.

Jan 1, 1979

By James R. Aggson

This Bureau of Mines report presents a finite element analysis of roof stresses associated with a 4-foot-high by 18-foot-wide underground coal mine entry. This analysis starts with known loading conditions determined in an underground coal mine in West Virginia and is extended to other possible underground loading conditions. The roof failures predicted by the finite element analysis under known loading conditions correlate well with the roof failures observed underground. The most probable failure modes are identified for the various loading conditions considered. Various failure preventive measures are discussed.

Jan 1, 1979

By P. C. Good

This Bureau of Mines report describes the preparation of phosphoric acid directly from phosphate ore, without prior beneficiation, in a small-scale, continuous process research unit, as part of an effort to improve minerals and metals recovery from domestic resources while minimizing environmental effects. Three phosphate-matrix samples, ranging in grade from 18.2 pct P20S5to 11.9 pct P205, were dry-fed at a rate of 1.82 kg/hr (4 lb/hr) to a continuous-circuit, 12-liter, single-tank digester to yield phosphoric acid and byproduct gypsum filter cake. Comparison with earlier data shows that a significantly improved filtration rate was attained in a single-tank reactor compared with that attained in a five-tank reactor train processing the same ore. Iron and aluminum impurities in the product phosphoric acid averaged about 60 pct higher than amounts reported in commercially prepared, concentrate-derived acid. All gypsum filter cakes prepared had a firm, sandy texture, rendering them physically suitable for stacking or landfill use. Introduction of dry attritioning and air classification approximately doubled the attainable filtration rate when the dry-beneficiated product was digested. In air classification, there was a 12-to 14-pct P205 loss. Depending on the technique used and the matrix grade, overall P205 recovery ranged from about 72 to 89 pct.

Jan 1, 1979

By L. A. Haas

The U.S. Department of the Interior, Bureau of Mines, is conducting laboratory-scale research to determine the leaching conditions required with sulfuric acid for extracting base metal from a matte with a copper-to-nicke1 ratio of 6 to 1. The matte (61.2 pct Cu, 9.7 pct Ni, 3.3 pct Fe, 21 pct S, and about 5 oz of precious metals per ton) was prepared from Duluth Complex (Minnesota) ore by smelting a bulk sulfide flotation concentrate. The matte was pre leached at atmospheric pressure to selectively extract 20 pct of the nickel, and the undissolved solids were referred to as the matte residue. Autoclave leaching of the matte residue extracted over 95 pct of the nickel, copper, and iron. The remaining leach residue in the autoclave contained over 100 oz of precious metals per ton. The leaching conditions required were matte grind of greater than 98 pct minus 325 mesh, pulp concentration of 50 g/1, total pressure of 100 psig with oxygen at 150° C or 400 psig with air at 180° C, 50 g/1 H2S04, 700 rpm agitator speed, and 6 hours of leaching time. The leaching time was decreased to 2 hours by increasing the agitator speed to 1,300 rpm. Sulfuric acid concentration greater than 50 g/1 did not appreciably enhance the base metal extraction, but with less acid, residues with higher iron concentrations were obtained. Supersaturation of the liquor was prevented at 150° C by using a 1ixiviant that contained 30 g/l Ni and 20 g/1 Cu.

Jan 1, 1979

By W. N. Cathey

Many materials including carbides, silicides, phosphides, borides, nitrides, oxides, and metals were studied by the Bureau of Mines as potential fuel cell catalysts for electroreduction of oxygen in a 1[N]H2S04 electrolyte. The objective of this study was to assess the potential of abundant, low-cost materials as substitutes for platinum or to increase the catalytic efficiency of platinum. Several compounds were rejected because of their reaction in the corrosive environment of the oxygen electrode. However, some of the remaining were the most active catalysts. Activity of carbides such as tungsten carbide could be improved by doping with platinum-group metals, by varying stoichiometry, or by sputtering on a layer of platinum. While no catalysts were found with activity as high as platinum, some compounds were shown to be deserving of further investigation.

Jan 1, 1979

By T. E. Bernard

The CO2-absorbent canisters used in four approved rescue breathing apparatus were investigated. A breathing machine was used to simulate human expiration with gas flow rates of 26, 37, and 48 1/min of 3.5% CO2 in air. The exit gas CO2 concentration, the pressure drop across the canister, and the exit-gas temperature were monitored. The absorbent capacities of the packed-bed canister designs were found to be dependent on flow rate within the range studied, while the capacities of the other designs were less affected. The radial canister had the least resistance to breathing while the complex bed design proved to be the most effective in utilization of the chemical. The overall results indicated that LiOH (lithium hydroxide) has the highest capacity for CO2 absorption among the absorbents tested. It can be used in a simple packed-bed design while maintaining acceptable levels of resistance and exit-gas temperature. Examination of oxygen supply with respect to CO2-absorption capacity suggested that it is desirable to closely match CO2-absorption capacity with the avail-able O2 supply to minimize the size and weight of rescue breathing apparatus.

Jan 1, 1979

By D. E. Shanks

As part of its goal to help maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines, U.S. Department of the Interior, is investigating a fused-salt electrolytic procedure for producing zinc metal. A previous report described preliminary, small-scale work on the fused-salt electrolysis of ZnC12. The present report covers a more detailed investigation of the properties of ZnC12-alkali metal chloride electrolyte systems in relation to the production of zinc metal and also discusses electrolysis in largescale, internally heated cells. The effect of composition on bath stability, current efficiency, cell voltage, and liquidus temperature was determined for the ZnCla-NaC1-KC1, ZnC12-NaC1-LiC1, and ZnC12-KC1-LiC1 electrolyte systems. An electrolyte com-posed of 38 mole-pct ZnC12, 31 mole-pct NaC1, and 31 mole-pct KC1 gave the best overall results. Sludge (ZnO) formation in the ZnC12-NaC1-KC1, ZnC12-KC1-LiC1, and ZnC12-KC1 systems was investigated during prolonged electrolysis. The ZnC12-KC1-NaC1 electrolyte showed the least sludge formation. A 1,500-amp cell was operated using the ZnC12-NaC1-KC1 electrolyte at 500° C. Zinc metal was produced at the rate of 4.0 lb/hr with a current efficiency of 95 pct.

Jan 1, 1979