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By D. E. Kirby

In line with the Bureau of Mines' goal of providing technology to maintain a supply of minerals adequate to meet national economic and strategic needs, a method for recovering chromite from lateritic materials was investigated. Laterites are a large resource of Ni, Co, and Cr, critical metals of which the United States has insufficient domestic sources. A roast-leach method was developed by the Bureau to extract nickel and cobalt from domestic laterites. A concurrent effort was made to recover chromium from either unprocessed laterites or the leach residues. This report characterizes laterites and laterite leach residues. It describes a chromite recovery procedure using conventional industrial beneficiation equipment for sizing, low-intensity magnetic separation, and gravity concentration. Concentrates containing 20.0 to 22.4 pct Cr (29.0 to 32.7 pct Cr203) and with a 1.6:1 to 1.9:1 Cr-Fe ratio were recovered from laterites and residues containing 1.3 to 2.5 pct Cr with recoveries exceeding 50 pct. Because of their low grade and fine size, these concentrates would be suitable for preparing chromium chemicals. The direct beneficiation of laterites for chromite recovery resulted in the minerals containing nickel and cobalt concentrating in slime products. No iron oxide coproducts of acceptable grade were recovered from either laterites or residues.

Jan 1, 1982

By R. L. Rickel

The Bureau of Mines, as part of its minerals environmental technology research, conducted a study of mine waste tailings disposal. Part of the investigation evaluated the sand bed dewatering technique for disposal of alumina mini plant tailings as a means to increase consolidation rates and contain effluents. The technique employs a bed of sand resting on an impervious bottom. The tailings slurry is impounded over the sand layer and is dewatered through bottom drain piping. The study employed a single 10-ft-high, 6-in-diam, clear polyvinyl-chloride (PVC) column, and thickener wastes from the acid leaching of calcined kaolin clay. Results showed a consolidation rate of 41 in in 186 days for a total volume reduction of 37 pct. Sand bed dewatering was an efficient technique for solid consolidation and effluent containment when compared with data obtained from other dewatering studies.

Jan 1, 1982

By Robert W. Waytulonis

The Federal Bureau of Mines contacted 29 organizations--mine maintenance departments and equipment manufacturers--concerning service experience and construction of diesel exhaust-gas water scrubbers. Scrubbers are used primarily on mobile diesel-powered mining equipment subject to 30 CFR 36. Because the scrubbers cool exhaust gas and act as flame arresters, their failure would compromise safety in underground mines. Scrubber maintenance problems and frequency and modes of failure were identified, and construction materials and techniques were evaluated. Three failed scrubbers were randomly selected from two cooperating mines, and their modes of failure were determined. In conjunction with failure analyses, mine water and scrubber water solution samples were chemically analyzed to characterize corrosive properties. Sludge and mineral deposits and different types of corrosion and metal fatigue were identified as problems leading to scrubber failure. The corrosion process is explained; maintenance practices, construction materials, and manufacturing methods that could be used to reduce premature failures and allow longer effective scrubber life are identified; and basic changes in scrubber design are suggested. If type 304 stainless steel is used throughout the scrubber and regular maintenance is performed, long, dependable service can be expected. Other materials such as 304L, 316, or other more exotic steel alloys may be necessary under certain conditions.

Jan 1, 1982

By T. J. Driscoll

Methane-air mixtures can ignite as a result of sparking or rubbing of materials, particularly by impact involving light alloys and rusted steel where an exothermic thermite reaction can occur. This report reviews the published literature and describes a new method utilized by the Bureau of Mines for studying the processes occurring during collisions of light metals with rusted steels. The method involves measuring the spectra of sparks and explosions in methane-air mixtures using a photodiode array. Initial results obtained using magnesium and aluminum alloy 6061-T651 projectiles striking rusted steel are reported. These results indicate that the continuous parts of the spectra show a larger intensity for incendive sparks compared with nonincendive sparks, with the largest relative change in the higher energy, ultraviolet region. An unexpected shift of the intensity maximum for the continuous parts of the spectra towards the infrared region was observed for the more incendive sparks. Evaluation of rusted steel samples with electron microscopy, energy-dispersive X-ray spectrography, and Auger electron spectroscopy after they had been impacted by aluminum alloys indicated that aluminum was transferred to the steel in the form of islands that became larger as a function of increasing projectile velocity.

Jan 1, 1982

By Arthur V. Petty

In Bureau of Mines research on recycling chrome-containing refractory wastes, used refractories from argon-oxygen decarburization and electric steelmaking furnaces were beneficiated. By means of dry magnetic separation on minus 6-mesh crushed wastes, a concentrate was produced. After minor adjustments to the particle size distribution, full-size refractory brick were dry-pressed by a commercial producer and fired to 1,450° and 1,730° C. Standard testing procedures were used to determine the cold-crushing strength, modulus of rupture at 25°, 1,300°, and 1,500° C, hot load, thermal shock resistance, thermal expansion, and slag resistance. Optical and electron microscopy were used to determine grain-bonding mechanisms, and energy-dispersive analysis of X-rays was used to determine elemental distribution. The test results indicate that the beneficiated material could be used to produce a refractory product suitable for moderate-temperature applications.

Jan 1, 1982

By R. O. Dannenberg

The Bureau of Mines conducted laboratory batch and small-scale continuous tests to remove traces of dissolved molybdenum from water simulating waste discharged from a molybdenum concentrator, Molybdenum concentrations, initially ranging from 2 to 10 ppm, were decreased to 0.5 ppm or less by coprecipitation of the molybdenum with freshly precipitated ferric hydroxide" The precipitate was separated as a froth by dissolved-air flotation for subsequent disposal. Although the treated water met current environmental standards for contained molybdenum, contained particulate iron might have to be removed by filtration for the water to be acceptable. Estimated costs for treating concentrator effluent water were 55 cents, 57 cents, and 64 cents per 1,000 gal at initial molybdenum concentrations of 2, 4, and 10 ppm, respectively.

Jan 1, 1982

By J. I. Paige

As part of a continuing effort to develop technology that maximizes mineral and metal recovery from domestic resources, the Bureau of Mines investigated a method to totally utilize copper converter slags without recycling them back through the matte smelting furnace. The research was directed toward (1) recovering the contained copper in converting slags by producing a recyclable copper-iron matte, (2) carbothermically reducing the slags to recover the iron, and (3) producing slag wool from the depleted slags. This report deals with the reduction of three industrial converting slags, containing 2.0 to 7.3 wt-pct Cu, in an 800-kVA electric arc furnace to produce a recyclable copper-iron matte. The addition of sufficient iron pyrite to provide 29 to 113 pct of the stoichiometric sulfur (based on producing 40-pct-Cu matte) produced a recyclable matte (36 to 61 pct Cu) at an energy consumption of 520 to 700 kWh per ton of solid material charged. The expected energy saving for treating molten slag in an electric furnace (5-to 9-MVA range) is about 400 kWh per ton of molten slag treated.

Jan 1, 1982

By E. Morrice

As part of its efforts to maximize process efficiency and decrease energy requirements in mineral processes, the Federal Bureau of Mines has investigated methods for beneficiating bastnäsite ores from Mountain Pass, Calif. The results of a bench-scale study on the flotation of bastnäsite ore are presented. Flotation at a pulp temperature of 40° to 45°C yielded a cleaner concentrate containing 58.7 pct RE203 at a rare-earth recovery of 67 pct. These results are comparable to those reported for the commercial beneficiation method in which the pulp is heated to boiling before flotation. An attempt was also made to recover a barite flotation concentrate from the bastnäsite rougher tailing. Concentrates containing only 70 pct barite were obtained.

Jan 1, 1982

By H. H. Dewing

The Bureau of Mines constructed a process research unit (PRU) to demonstrate new technology for extracting zinc from sphalerite concentrates. Up to 9 kg/hr of sphalerite (ZnS) concentrate was reacted at ambient pressure in the PRU with 80 pct sulfuric acid at 160° to 180° C to produce zinc sulfate and elemental sulfur. The PRU consisted of a three-stage glass reactor system: a 4-liter premix stage in which feed was slurried with 78 to 82 pct H2S04, a 40-liter stirred reactor, and a ISO-liter settling stage in which high reaction conversions were effected and excess H2S04 for recycle was separated from insoluble ZnS04 and sulfur. Evolution of sulfur-containing gases was minimized by sub-surface addition of acid feed slurry to the stirred reactor and by exclusion of air from the reactor to prevent the oxidation of elemental sulfur. Conversion of zinc to zinc sulfate averaged over 99 pct at the optimum acid concentration of 80 pct. Total sulfur losses (primarily S02) were less than 2 pct of the sulfur in the sphalerite. Elemental sulfur remained in the insoluble portion of the settled reactor product after leaching with simulated spent zinc electrolyte containing sulfuric acid. The sulfur residue contained 75 to 89 pct sulfur. Neutral zinc sulfate, required for zinc electrowinning processes, was separated from the sulfuric acid leach solution by crystallization at -15° C as zinc sulfate heptahydrate (ZnS04?7H20). The crystallization operation simultaneously effected a partial concentration of the recycled electrolyte solution by removing water.

Jan 1, 1982

By William H. Pomroy

The Bureau of Mines, through a 4-year program of combined in-house and contract research, has developed the necessary hardware and software technology to provide rugged, reliable automatic fire protection for surface mining mobile equipment. One element of this program was a continuing effort to help foster rapid mining industry acceptance of the technology by keeping end user costs reasonable. This report is an analysis of the economic impact of surface mining mobile equipment fires and the cost benefit of utilizing automatic fire protection systems to abate these losses.

Jan 1, 1982

By Victor R. Spironello

The Bureau of Mines has conducted studies of the slags related to ferrous technology to evaluate experimentally acceptable substitutes for the auxiliary flux, mineral fluorspar, in steelmaking operations. Comparative heats were made in a 1/4-ton, pilot-scale, basic oxygen furnace (BOF) to evaluate a waste material known as "used potlining." Used pot lining is recovered from alumina reduction cells after its useful life and contains significant levels of fluorine and sodium in various compounds. This material in both lump and pelletized form provided adequately fluid slags, based on observations made during BOF operation. No adverse effects were found on furnace performance, metal and slag chemsitry, the strength of the steel produced, or the environment. Fluorine recovery in the slag was about the same as that obtained when using fluorspar, as were the losses to the scrubber water and solids. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag. The sodium recovered in the slag apparently also contributed to fluidity, since the fluorine input was at about two-thirds that of the fluorspar. Used potlining was determined experimentally to be a satisfactory substitute for fluorspar in basic oxygen steelmaking.

Jan 1, 1982

By Richard J. Mainiero

The Bureau of Mines conducted research to evaluate the optimum design for a rock-breaking explosive charge that could be fired unconfined in a gassy or dusty coal mine without the danger of igniting the flammable atmosphere. Charges of various shapes, with and without cavities, were tested in a gallery using 3-by 3-by l-ft concrete blocks as simulated boulders. For these tests the optimum charge, in terms of cost, weight, and convenience in handling, consisted of a flat l-1/2-lb charge of permissible explosive seven-eighths of an inch thick and 7 in in diameter encased in a l/2-in thick layer of fine salt (NaCI). This work demonstrated that it should be possible to produce an inexpensive explosive rock-breaker charge that would be safe to use in underground coal mines.

Jan 1, 1982

By Jack C. White

As part of an investigation of the production of alumina by the nitric acid leaching of kaolinitic clay, the Bureau of Mines designed, built, and tested a fluidized-bed system for the calcination of aluminum nitrate nonahydrate to alumina, while recovering nitric acid. The calciner consisted of an 8-in-square by 36-in-tall vessel containing 18 in of fluidized solids. Molten aluminum nitrate, sprayed directly into the fluidized solids, formed sandy, granular alumina by growth of successive layers on fluidized particles. Solids were fluidized in a dense bed at temperatures of 250° to 500° C with steam, air, or mixtures thereof. Decomposition of nitrate ranged from 4 to 10 pet during single-pass steam or air fluidization, respectively. Alumina dust losses and low throughput are significant unsolved problem areas.

Jan 1, 1982

By D. S. Burgess

About 100 tests of flammability were carried out with H2, CH4, and CO in mixtures with air using the Federal Bureau of Mines 12-ft-diameter spherical pressure vessel as an explosion test chamber. The LeChatelier approximation gave slightly conservative estimates of the limits of downward flame propagation (onset of significant pressure rise) using the following measured values for the individual gases, in percent: H2, 8.5; CH4, 5.25; CO, 13.0. No justification could be offered for using the LeChatelier law for upward flame propagation limits and indeed reported data suggest that calculated values would not be conservative. The observed upward limit for methane-air mixtures (4.85 pct) was less than the widely accepted lean limit for this fuel; those for lean hydrogen-air mixtures and carbon monoxide-air mixtures did not differ from the lowest accepted values. Diffusional effects on the propagation of single, binary, and ternary fuel mixtures are discussed.

Jan 1, 1982

By John L. Schaller

The Bureau of Mines, U.S. Department of the Interior, has investigated the extraction of alumina from domestic kaolin clay by leaching with boiling 26 wt-pct hydrochloric acid. Acid leaching of crushed calcined kaolin feed yields slurries that are slow settling and difficult to filter because of the presence of fine particles generated in crushing, calcining, and leaching. Laboratory research showed that tumbling and moistening crushed raw kaolin on a pelletizing disk caused the fines to agglomerate on the surfaces of the larger particles, while the sharp edges and corners of the larger particles were rounded off. Minus 16-mesh crushed raw kaolin was misted on a 36-in-diam, 8-in-deep pelletizing disk at rates of 175 to 250 lb/hr, and was calcined in either a rotary or a fluidized-bed calciner; negligible degradation occurred. The physical properties of the misted calcined kaolin were evaluated in the leaching system of the clay-hydrochloric acid miniplant. Only minor attrition occurred during leaching, and the slurry was readily filtered on a continuous belt filter.

Jan 1, 1982

By Masami Hayashi

The Bureau of Mines conducted laboratory studies to investigate methods for desilicating sodium aluminate solution derived from leaching a limestone-anorthosite sinter with 10-pct Na2C03 solution. Desilication tests were made at atmospheric pressure to determine the effects of time and additions of lime and desilication residues. A two-stage, countercurrent desilication procedure was developed to reduce the Si02 content sufficiently to meet specifications for cell-grade A1203. Both stages were conducted at boiling temperatures at atmospheric pressure. Reagent lime was charged as desilication seed to the partially desilicated solution in the second stage, and a product (desilication residue) precipitated by the lime addition was charged to the freshly leached solution in the first stage. Average A1203 loss in the desilication circuit was 5.8 pct, and the product solution contained less than 0.04 g/l Si02. Complete precipitation of A1203 by carbonation resulted in a hydrate containing less than 0.01 pct Si02. Calcination of this hydrate would produce A1203 meeting the 0.015 pct Si02 specification for cell-grade material.

Jan 1, 1982

By V. E. Edlund

As part of a research program for recovering alumina from domestic nonbauxitic resources, the Bureau of Mines investigated a lime-sinter, caustic leach technology for anorthosite. This report discusses the unit operations--feed preparation, sintering, and leaching. Acceptable pellets for the bench-scale sintering studies were prepared from mixtures of minus 200-mesh anorthosite and limestone using water alone as the pelletizing agent. Heating pellets at 1,270° to 1,360° C for periods of 0.5 to 2 hr, followed by a 15-min soaking period at 700° C and cooling to room temperature, produced a sinter that dusted to more than 90 pct minus 65 mesh. The weight ratio of limestone to anorthnsite was critical in producing sinter exhibiting good dusting and leaching characteristics. A ratio of 2.0 was optimum for the bulk samples of anorthosite and limestone used in this research. Leach solutions from lower ratio sinters were unstable; gelation became progressively more severe with higher ratio sinters. Leaching the dusted sinter with 10-pct Na2CO3 at 60° C extracted 85 to 90 pct of the alumina in a product solution containing about 50 g/l A1203. Leach residue in contact with pregnant solution tended to set up as a rigid gel as a result of cementation, comp action, and gelation. The presence of a calcium-sodium zeolite [(Cn,Na2)6?(Al2Si04)12?27-3OH20] in the ungelled residues seemed to be the main difference between gelled and ungelled residues.

Jan 1, 1982

By R. Emmett Hughlett

The Bureau of Mines has developed a statistical approach to the laboratory evaluation of response bias and precision in gas detectors. The techniques described employ a computerized analysis and a new method of data presentation called composite graphing. The underlying theory, its practical application to the data, and the experimental equipment and procedure are described.

Jan 1, 1982

By J. M. Gomes

Bench-scale flotation tests were conducted on two western tactite ores to study the recovery of tungsten and zinc minerals. The investigation, which is part of the Bureau of Mines ongoing program to develop methods for beneficiating minerals and metals from domestic low-grade ores, demonstrated the feasibility of producing scheelite, sphalerite, and their bulk concentrates. Sphalerite concentrates containing 51 to 53 pet Zn and less than 0.11 pct W03 were selectively recovered prior to scheelite flotation. Zinc recovery ranged from 85 to 91 pct. Scheelite concentrates containing 17 to 25 pct W03 were then recovered from the ore; tungsten recoveries ranged from 88 to 94 pct. Bulk flotation concentrates containing 84 to 91 pct of the W03 and 87 to 95 pct of the zinc also were prepared. More than 98 pct of the W03 in a bulk concentrate containing 9 pct W03 was extracted by autoclave leaching with a soda solution. The zinc remained in the leached residue.

Jan 1, 1982

By E. G. Baglin

As part of an effort to decrease U.S. dependence on imports of critical and strategic metals, the Bureau of Mines investigated three leaching methods for extracting the base metals and recovering platinum-group metals (PGM) from matte prepared from Stillwater Complex flotation concentrates. Because of a limited supply of natural material, synthetic matte of composition similar to matte prepared from natural concentrates was used to devise the extraction sequences. The validity of the sequences was verified with matte prepared from Stillwater concentrates. In two-stage matte leaching, first-stage H2S04 leaching extracted 99 pct of the nickel and iron from the matte but negligible amounts of copper and PGM. Second-stage oxidative leaching with Fe2(S04)3 or FeC13 solubilized more than 98 pct of the copper and no precious metals. Sequential leaching, in which acid and oxidizing lixiviants were added sequentially to the matte without an intervening filtration step, extracted 99 pct of the Fe, Ni, and Cu. A roasting-leaching technique, in which the residue from first-stage leaching was roasted between 360° and 500° C before a second leaching with H2S04, solubilized 98 pct of the copper. The three leaching methods yielded high-grade PGM residues containing more than 98 pct of the PGM in the matte.

Jan 1, 1982