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By T. H. Jeffers

The Bureau of Mines conducted laboratory tests to devise a procedure for extracting copper from low-grade discarded mill tailings. A solid extractant consisting of an organic solvent extraction reagent adsorbed on granular activated carbon was investigated and proved to be satisfactory for extracting copper directly from leach pulps. When this material was used in a cyclic leaching, stripping, and electrowinning pro-cess, 95 pct of the acid-soluble copper was recovered from oxidized mill tailings. The weathered tailings contained 0.24 pct Cu (total) and 0.20 pct acid-soluble Cu. The copper was recovered as cathodes containing, in parts per million, 1.6 Pb, 3.6 Fe, 0.5 Sb, 1.5 AI, 1.9 Mn, and <1 Mg.

Jan 1, 1985

By R. Blickensderfer

Laboratory wear testing was conducted by the Bureau of Mines on a variety of typical wear-resistant alloys used in mining and mineral-processing equipment to establish their relative spalling and abrasion resistance. Test specimens in the form of 75-mm-diam balls were subjected to repeated impacts until they broke, spalled excessively, or received several hundred thousand impacts. Pin specimens removed from the balls were evaluated for high-load abrasive wear. The alloys in-cluded commercial forged steels, cast steels, manganese steels, and four types of white cast iron, with a range of heat treatments. The effects of hardness and microstructure on impact wear and abrasive wear are discussed. The data should help mine operators select the compositions and heat treatments that best suit service conditions.

Jan 1, 1985

By E. G. Baglin

The Bureau of Mines devised a procedure for selectively extracting platinum-group metals (PGM) and gold from Stillwater Complex flotation concentrate. The Stillwater Complex is the only major U.S. PGM resource. Development of a suitable extraction technique will contribute to its exploitation. The concentrate was roasted at 1,050° C to convert host base-metal sulfides to oxides and the PGM from sulfide minerals to their elemental states. The roasted concentrate was preleached with dilute sulfuric acid to remove easily soluble gangue minerals. After pre-leaching, the concentrate was slurried with 6M HCI and leached at ambient temperature and pressure with a strong-oxidizing agent. Hydrogen peroxide, chlorine, sodium hypochlorite, nitric acid, and a persulfate salt were the oxidants investigated. The two-stage leaching scheme ex-tracted up to 97 pct of the platinum, 92 pct of the palladium, and 99 pct of the gold from the roasted concentrate. The base metals were not solubilized and reported to the residue. No attempt was made to devise a procedure to recover the copper and nickel because they comprise less than 5 pct of the value of the concentrate. Viable techniques for recovering the precious metals from the pregnant solution were sulfide precipitation, cementation with nickel, or adsorption on activated carbon.

Jan 1, 1985

This Bureau of Mines investigation addressed two primary issues of air velocity measurement in mines: the determination and use of correction factors, and the development of guidelines for the selection of a suitable site at which the measurements should be taken. Other facets of the investigation included a comparison of measurement methods and devices, and aircourse cross-sectional area measurement. The study consisted of theoretical, laboratory, and in-mine investigations. The measurement devices included in the experimental phase were vane anemometer, vortex shedding anemometer, a prototype thermoan-emometer, smoke tube, and oil of wintergreen sprayer. The measurement methods included single-point centerline, timed-point traverse, continuous traverse for the anemometers, and various distances and cloud positions for the smoke tube and oil of wintergreen devices. The study resulted in guidelines for measurement site selection that are applicable to most inmine situations. It also showed that the use of correction factors is problematic. There are many potential pit-falls and there are cogent arguments against using certain correction factors. However, generalized correction factors were developed that can be successfully applied in routine ventilation work, provided that their use is properly understood.

Jan 1, 1985

The objectives of this research were to examine and to laboratory performance of several brands of rigid urethane een brands, produced by 13 manufacturers, were examined. was performed in a laboratory under controlled conditions. document the foam. Eight-All testing Preliminary laboratory tests included flame spread evaluations, flame penetration, ignition temperatures, air permeability, and adhesion. Having established arbitrary cutoff values, the original 18 candidates were narrowed to 8. More specialized tests followed. The effects of water immersion and dry aging on flame spread performance and other physical properties were then examined. This Bureau of Mines report was written to provide information for those concerned with using rigid urethane foam as a sealant. Its intent is to describe the various laboratory evaluations performed and to delineate the performance of each candidate. This report neither promotes nor discourages the use of rigid urethane foams. It presents results that will enable those responsible for using or enforcing the use of rigid urethane foams in underground mines to make informed decisions.

Jan 1, 1985

By C. W. Huggins

The objective of this Bureau of Mines research was to compare the size distribution of respirable quartz collected at coal mines with that of several reference standards used to quantify quartz in coal mine dust samples. Particle size measurements were made on 23 samples and 4 ref-erence standards using a scanning electron microscope in the backscatter electron mode of operation, interfaced with an image analysis system. The Mine Safety and Health Administration provided the 23 respirable coal mine dust samples, which were collected at surface and underground coal mines in 7 States. The accumulated particle size measurements in-dicate three of the reference standards, minus 5-um Min-U-Sil, minus 5-um Supersil, and NBS 1878, would be preferred over the fourth, Silver Bond B, for quantitative quartz determinations in coal mine dusts by X-ray diffraction and infrared spectrometry.

Jan 1, 1985

By S. S. M. Chan

The Bureau of Mines has investigated the structural aspects of shafts and support systems using the finite-element technique. In situ field measurements in deep, vein-type metal mines show that rock stresses are often higher in the horizontal direction than the vertical, and unequal in the horizontal plane. These data and laboratory and field-determined physical properties were used as input to analytical studies. Various design and construction parameters were investigated to deter-mine the effect on shaft stability. Rectangular shafts were studied in detail to determine the effects of applied stress ratio, shaft orientation and dimension, influence of interbedded quartzite and argillite, and rock fracturing. Various support systems were analyzed, including concrete lining, timber, and steel sets. Circular configurations were investigated to evaluate yield zones and liner thickness. Elliptical shafts and time effects were briefly evaluated to illustrate shape and time effects and demonstrate the methodology. It is shown that the magnitude, direction, and ratio of applied stress and rock mass anisotropy are keys to determining shaft stability. A realistic conceptual framework was developed with which to examine the rock and support interaction in deep mine shafts. Structural analysis techniques overcome some of the historical difficulties with shaft de-sign by defining the field data requirements and structural sensitivity of various design and construction parameters.

Jan 1, 1985

By Gary L. Hundley

The Bureau of Mines has devised a procedure to recover chromium chemicals from low-grade domestic chromites, which contain silicon and aluminum impurity levels that are too high to permit processing by present industrial processes. The Bureau procedure consists of reacting chromite with molten sodium hydroxide (NaOH) under oxidizing conditions to form sodium chromate (Na2Cr04). The reaction product is leached with methanol to remove the majority of the unreacted sodium hydroxide, then with water to remove the sodium chromate and the remainder of the sodium hydroxide. The sodium chromate product is recovered by evaporative crystallization from the aqueous solution. This report presents results of laboratory tests to determine the optimum fusion conditions and the chromium extractions obtained from several domestic chrotdte concentrates. These concentrates are from a variety of sources, including the Stillwater Complex in Montana, Kanuti River-Caribou Mountain, Red Bluff Bay, Kenai Peninsula, and Kodiak Island areas in Alaska, deposits in northern California, and a nickel-cobalt laterite from southern Oregon. All of these concentrates were successfully treated by the Bureau procedure. The best chromium extrac-tions obtained for each of these materials ranged from 69.5 to 98.9 pet.

Jan 1, 1985

By D. L. Sawyer

The Bureau of Mines studied alumina extraction from uncalcined, kao-linitic clay at temperatures from 1000 to 2500 C using 20-or 27-wt-pct-HCI concentrations and with an acid-to-clay ratio of from 0.8 to 1.4 times stoichiometric. Autogenous digestion pressures ranged from atmospheric pressure to about 900 psia. Extraction of 96 pct of the alumina was obtained by HCI leaching at temperatures and leaching times that varied from 1000 C for 120 h to 2000 C for 15 min. Hydrochloric acid stoichiometry of the reaction A1203&apos;2Si02&apos;2H20 + 6HCI + 2AICl3 + 2Si02 + 5H20 was studied at different temperatures and leaching times in a 750-mL tetrafluoroethylene-polymer-lined autoclave. A combination of high temperature and 20 wt pct excess HCI promoted rapid and almost quantitative extraction of alumina (99 pct in some tests). Additional Bureau data obtained with 35-mL tantalum bombs and leach-ing tests with added fluoride are also provided. At high temperatures, the addition of fluoride did not result in a significant improvement over HCI alone and was deleterious to the filtering properties of the digest residue.

Jan 1, 1985

By James P. Bennett

The Bureau of Mines investigated the effect of refractory oxide additions, introduced in soluble form, on the high-temperature properties of 90- and 98-pct-MgO brick. Brick samples were soaked in solutions containing Al, Ca, Cr, Co, Fe, Mg, Mn, Mo, Ni, Si, Sr, Sn, Ti, or Zr ions. Additions to 98-pct-MgO brick did not generally result in statistically significant property improvements. Statistically significant improvements were noted in hot modulus of rupture (MOR), slag resistance, and spalling resistance of the 90-pct-MgO brick for additions of Al, Mg, or Sn. High-temperature performance of treated 90-pct-MgO refractories was equal to or approached that of 98-pct-MgO brick. The marked improvements due to tin were obtained with additions of only 1.14 wt pct Sn02.

Jan 1, 1985

By J. F. McIlwain

Cobalt-base hardfacing alloys used for wear resistance consist almost entirely of metals largely imported into the United States. As part of an overall research program to help alleviate this foreign dependency, the Bureau of Mines has been investigating an iron-base alloy system as a potential replacement for cobalt-base alloys for some uses. To ascertain the melting ranges, thermal analyses were made of cast heats of alloys containing, in weight percent, 59-61 Fe, 16-19 Cr, 8-9 Ni, 1 Mn, 1 W, 1 Mo, 0.5 Cb, 0.6 Si, 0.3 C, and 0-12 stoichiometric TiB2. Powder alloys within this range of composition, prepared by mechanical alloying, were sized and applied to mild steel test coupons by nontrans-ferred-arc plasma spraying. The resulting thin coatings were >95 pet dense, with bond strengths of 35 MPa and hardness of 400 to 840 DPH. Abrasive and adhesive wear test data were compared to those of a plasma-sprayed cobalt-base alloy. A range of boride contents resulting in most promising properties was determined for further research.

Jan 1, 1985

By M. Hertzberg

The Bureau of Mines measured the energy requirements for the spark ig-nition in air of Pittsburgh seam bituminous coal dust, lycopodium spores, and polyethylene powder with a 1.2-L furnace and 8-L and 20-L chambers. Thermal autoignition temperatures of the same dusts were mea-sured in the 1.2-L furnace. Electrical ignition requirements are given in terms of both effective spark gap energies, [ ] and stored circuit energies, 1/2 CE2. The measured order of electrical ignitability for the three dusts is consistent with the data of other researchers; however, the absolute values are systematically higher, probably because of higher flow and turbulence levels in the chambers used and lower electrical efficiency in the circuit used here. The temperature dependence of the lean limit of flammability for lyco-podium was measured wi th the 1.2-L sys tem, and those measurements con--firm the applicability of the modified Burgess-Wheeler law to a dust. Due to experimental complexities, the minimum ignition energies for dusts may not reflect intrinsic flammability behavior. However, some valuable information may be obtained from the relative ignition energies of various dusts at ambient and elevated temperatures. In addition, the concept of minimum electrical ignition energies for homogeneous gas mixtures is reevaluated theoretically.

Jan 1, 1985

By J. D. Dixon

This Bureau of Mines report describes the results of an investigation for developing and applying procedures for stabilizing excavations openings in highly yielding ground. The approach developed in this report involves nonlinear modeling of the progressive relaxation of the zones of rock mass around the excavations opening where Coulomb criterion of failure is exceeded. Stresses are calculated by using a computer code; Coulomb-failure condition is examined for both intact rock and joints (using strength parameters [~] and c). The rock mass in the failed zones is relaxed by reducing the Young&apos;s modulus of the rock based on an empirical formulation that is a function of the shape of the opening and the extent of the failed zone. In addition, the material in the failed zone is assigned reduced strength paramters 0&apos; and c&apos;. The limiting (or convergent) relaxed zone is obtained through an iterative process by manually changing the rock modulus and the strength parameters between iterations. Support pressures are computed by applying forces normal to the excavation surface. The approach is applied to the analysis of stability and support requirements for an entry in a longwall coal mine.

Jan 1, 1985

By Jon C. Volkwein

The Bureau of Mines, Foster-Miller Inc., and Beaver Creek Coal Co. have evaluated the ability of a new system to ventilate a 40-ft-deep cut. A remote-control continuous-mining machine, in a 7-ft-thick seam, with exhausting brattice was fitted with an improved sprayfan system plus additional forward and reverse pointing sprays. Static and dynamic tests using tracer gas were conducted in a full-scale model and under-ground to measure the effectiveness of exhaust face ventilation for various deep-cutting mine and spray configurations. When compared to a lO-ft primary ventilation brattice, the extended-cut spray system consistently provided better face ventilation at all configurations up to and including a 40-ft brattice setback. The system also provided good dust protection and visibility for the machine operator. Another safety advantage is the elimination of the need to set temporary roof supports to maintain the ventilation brattice.

Jan 1, 1985

By F. J. Palumbo

Effective recycling or disposal of flue dusts is a continuing problem for copper, brass, and bronze smelters. Over 300,000 short tons (st) of dust is generated annually by U.S. secondary copper, brass, and bronze smelters. The Bureau of Mines has developed an alkaline leach method for recovering metal values from copper converter flue dust containing zinc, tin, lead, and copper. The dust was leached with a hot solution of ammonium chloride and ammonium hydroxide to solubilize ZnO. All of the tin (as Sn02) and the metallic copper, lead, and zinc, as well as possible insoluble compounds of each, report to the residue. Dissolved copper and lead salts are removed from the leachate by cementation with granular zinc. Zinc oxide is precipitated by diluting the leachate with water. The tin-rich (9.8 pct) residue has a ready market. The cement product is recyclable to the smelting operation. The ZnO is at least 97 pct pure and has potential marketability.

Jan 1, 1985

By Larry A. Haas

The Bureau of Mines is investigating the use of complex gas mixtures, such as would be produced by coal gasification, for reducing iron oxide pellets. A semiempirical model was developed to predict a priori the reduction rate of an iron oxide pellet in a laboratory tube furnace with simulated coal gases at a total pressure of 1 atm. The model uses partial pressures of H2, CO, CO2, CH4 (methane), water vapor, and a temperature-dependent term to predict the rate of reaction. The reduction rate (weight loss per unit of time) was determined with a thermo-gravimetric apparatus (TGA) in the temperature range of 800° to 1,100° C. The ranking of the reductants, in order of decreasing reducing potential, is H2, CO, and CH4 at temperatures between 800° and 1,000° C; however, CH4 became a better reductant than CO at 1,100° C. Water vapor did not decrease the reduction rate as much as did CO2, Carbon deposition was observed at temperatures below 1,000° C with gas mixtures with high CO and low H2 concentrations. With low-Btu gas at 900° C, over 90 pct of the iron oxide was reduced to iron in less than 3 h. This com-pares with a reduction time of 1.5 h with medium-Btu gas and 1 h with reformed natural gases.

Jan 1, 1985

By Kim B. Shedd

The Bureau of Mines measured fiber dimensions on crocidolites (riebeckite-asbestos and magnesioriebeckite-asbestos) from the world&apos;s four crocidolite mining regions. The objective of the study was to determine whether there are measurable morphological differences between crocidolite fibers that correlate with the high reported incidence of mesothelioma in miners and mill employees in the Cape Province of South Africa and Western Australia, as compared with little or no reported incidence of this cancer in the Transvaal Province of South Africa or Bolivia. Fiber dimensions measured with the scanning transmission elec-tron microscope showed that crocidolites from Western Australia and the Cape Province have more thin fibers than crocidolites from Bolivia and the Transvaal Province.

Jan 1, 1985

By G. A. Smyres

The Bureau of Mines investigated a HCI-02 leaching procedure to recover Cu, Ni, and Co from a low-grade bulk sulfide flotation concentrate prepared from the Duluth gabbro complex. Since the Duluth gabbro complex is the largest known and unexploited Ni resource in the United States, the development of options for extracting the metal values from the flotation concentrate of this domestic resource is necessary. Conditions were determined for producing a pregnant solution low in Fe to facilitate recovery of the metal values. Leaching experiments were conducted at 15 pct solids, 1000 to 1200 C, 0.2 to 0.3 g HCI per gram concentrate in a 50-gal reactor pressurized to 50 pSig with 02. Base metal extractions from the concentrate were, in percent, 90 to 92 Cu, 99 Ni, 97 to 99 Co, and 0.1 .Fe. Precious metals extractions were erratic and unpredictable; at best their extractions were, in percent, 55 Au, 90 Ag, 40 Pt, and 45 Pd. The reaction time at 1200 C was 0.5 h. The use of compressed air instead of 02 as the oxidant was also investigated. Solvent extraction using LIX 622 was used to remove Cu from the pregnant solution. Cementation on Cu was tested for precious metals recovery, while sulfide precipitation was used to produce a Ni-Co product. A conceptual flowsheet for treating the Duluth gabbro concentrate is proposed.

Jan 1, 1985

By K. E. Soroka

More than 500 fires are now burning in abandoned coal waste banks and coal deposits in the United States. Once established, such fires can burn for decades, and extinguishing them by conventional methods such as surface sealing to exclude air, excavation to remove fuel, or flushing to cool the fire zone is usually difficult and always expensive. Burnout Control, a technique developed by the Bureau of Mines for the control of abandoned coal fires, involves the accelerated combustion of coal in place with total management of the heat and fumes produced. A burning waste bank or mine is placed under negative pressure relative to the atmosphere, and heat and combustion products are drawn from the combustion zone through an exhaust ventilation system. Heat produced appears as sensible heat in the exhaust, at temperatures as high as 1,0000 C (1,832° F), and could be recovered for the production of steam, hot water, process heat, or electricity. The Bureau&apos;s first held field demonstration of Burnout Control was at Calamity Hollow in Allegheny County, PA (near Pittsburgh). Calamity Hollow was the site of an underground mine in the 1900&apos;s and was surface mined in the 1940&apos;s. In the winter of 1961-62, a fire of undetermined origin was discovered in the exposed coal. In 1963, the Bureau constructed a trench barrier around the fire and a surface seal over the affected area. The fire was isolated but not completely extinguished. In 1979, when the Bureau began work on the Calamity Hollow Mine Fire Project to demonstrate controlled burnout, the fire was still smoldering on the hot side of the trench barrier. The project, which was begun in December 1979 and ended in July 1982, consisted of the design, construction, operation, and subsequent dismantling of a Burnout Control ventilation system. This report is the fifth in a five-part series that describes the Calamity Hollow Mine Fire Project. The first report, part 1, describes the design and construction of the field installation. Part 2 will present the results of a continuous 4-month burnout operation. (Because part 2 involves the analysis of a substantial body of data, it will not be published until after publication of parts 1, 3, 4, and 5.) Part 3 describes the instrumentation used to control and monitor the progress of the burnout operation. Parts 4 and 5 deal with the closeout phase of the field demonstration. Part 4 describes the procedure used to quench the fire, and this part (part 5) describes the final excavation and backfilling of the heated zones. The reports in this series document the Calamity Hollow controlled burnout demonstration which showed that (1) controlled in situ combustion is a feasible method for controlling underground fires in abandoned mines, (2) the resultant thermal exhaust output is sufficient for energy utilization, and (3) water injection-fume exhaustion is a potentially effective method for cooling large underground fire zones. Further investigations of both Burnout Control and the water-injection-fume exhaustion quenching procedure are planned.

Jan 1, 1986

By G. W. Elger

The Bureau of Mines investigated the conversion, at both laboratory and pilot plant scale, of a low-grade ilmenite to chlorination-grade feedstock that could substitute for imported rutile used to produce titanium tetrachloride. The concentrate was derived from the Tahawus, NY, lode deposit of ilmenite-magnetite in rock that contains anorthosite and gabbro. Charges of the ilmenite concentrate, containing 46.6 wt pct Ti02 blended with soda ash, were carbothermically reduced in an electric arc furnace, which separated most of the iron and left a high-titanium slag. However, the slag contained Ca, Mg, and Mn constituents that rendered the material unsuitable for continuous chlorination by causing plugging problems. After being ground and pelletized, the slag was reacted with S02 and air at 7000 to 9000 C, which selectively converted the harmful impurities to soluble compounds that were removed in a subsequent water or dilute HCI leach. In laboratory tests, the combined levels of harmful impurities were decreased from 5 to as low as 0.5 wt pct in leached slags. In pilot plant tests, leached slags sulfated at a rate of 10 lb/h averaged 85.5 wt pct Ti02 with pertinent impurity levels averaging 1.86 wt pct. The leached slag was successfully chlorinated in a laboratory fluidized-bed reactor at 9500 C to extract titanium as TiCI4.

Jan 1, 1986