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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 Stephen D. Cramer

The solubility of methane, carbon dioxide, and oxygen was measured in brines at temperatures from 0° to 300° as part of Federal Bureau of Mines research on the corrosion of metals in high-temperature geothermal and mineral processing environments. Solubilities were measured by the technique of extracting pure gas, dissolved at pressures where Henry's law was applicable, from known volumes of brine. The results were smoothed with respect to temperature. The solubility, expressed in terms of the Henry's law constant, reaches a maximum at temperatures ranging from 60° to 100° C for methane and oxygen, and from 160° to 170° C for carbon dioxide. The Henry's law constant increases, that is, gases are salted out of the brines, in the presence of dissolved salts. Salting-out coefficients are strongly dependent upon temperature. The temperature dependence of the Henry's law constant for geothermal brines is different from that for sodium chloride brines owing to the more complex chemistry of the geothermal brines. The solubility of oxygen and carbon dioxide in brines exposed to air saturated with water vapor and at a total pressure of 760 mm Hg is reported for temperatures from 0° C to the normal boiling point.

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 Durkin

The Bureau of Mines has conducted field studies in coal mines through- out the United States to determine the effectiveness of electromagnetic techniques in locating miners trapped underground following a mine accident. Data from these tests have been used to generate models of expected signal and noise distributions as found above mines throughout the coalfields. These distributions have aided in placing the expected performance of a through-the-earth electromagnetic communications technique into a probabilistic framework. Results show that at a 10-pct false alarm rate, the expected probability of detecting a miner's signal from a depth of 1,000 ft is 54 pct; at 500 ft it is 95 pct. These depths exceed the actual depths of 90 pct and 50 pct, respectively, of U.S. coal mines. Sensitivity studies have shown that at a depth of 1,000 ft, for every 3 db of improvement in signal-to-noise ratio, the probability of detection increases 6 to 8 pct.

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

By A. E. Raddatz

The Bureau of Mines is investigating methods for recovering tungsten from domestic resources. A calcine-quench-leach (CQL) technique was developed for the extraction of tungsten from the Golconda, Nev., hot springs ores. The deposit contains disseminated tungsten that cannot be beneficiated by conventional techniques and must be treated by hydro-metallurgical methods. The CQL procedure consists of calcining the ore at 900° C for 3 hours, quenching in a solution containing 1.5 parts of Na2C03 and 1.5 parts of NaOH per part of WO3 in the ore and at a solution-to-ore ratio of 3 to 1, leaching at 200° C and at 250 psig for 3 hours, and filtering and washing the residue. A series of closed-circuit batch tests showed that 92 pct of the tungsten was extracted from a sample containing 2.32 wt-pct W03. The pregnant solution contained 11 g/l W03.

Jan 1, 1982

By Sterling J. Anderson

To define the technical competence and capabilities of a nonexplosive excavation concept, the Bureau of Mines conducted reduced-scale laboratory tests of a mechanical excavation tool called a rock splitter. Hydraulically actuated splitters, capable of generating both radial and axial loads on a predrilled hole, were designed and fabricated. Through paired variable testing and drifting simulation, reduced-scale splitter performance was evaluated in concrete. Testing proved that the rock splitter is capable of excavating within the highly confined drift set-ting and that it offers a distinct advantage over splitters that can generate radial loads only.

Jan 1, 1982

By L. W. Higley

It is estimated that well over 20 million lb of chromium and 8 million lb of nickel, plus other metal values, are diverted annually to furnace dusts, mill scale, and contaminated swarfs in the domestic stainless and other specialty steelmaking industry. Little inroad has been made toward the in-plant recycling of these wastes to reclaim the metal values. The Bureau of Mines has devised a process for recovering about 90 pct of the chromium and molybdenum and well over 90 pct of the nickel and iron from stainless steelmaking furnace dusts, swarf, and mill scale. Other metals such as manganese are also recovered. Initial laboratory results were confirmed and expanded to include a wide variation of stainless steelmaking waste mixtures. Later experiments have included specialty steelmaking wastes other than from stainless steelmaking. Significantly, the ease of technology transfer has been demonstrated by a number of industrial-sized (19-ton) commercial electric furnace heats, in which the pelletized wastes represented some 10 to 20 pct of the furnace charge, replacing part of the normal scrap charge. Results of these successful large-scale trials are presented. Some information is also presented on incorporation into the pellets of chromium-bearing particulate wastes originating from other than steelmaking production. Cost evaluation indicates the process is economically attractive.

Jan 1, 1982

By J. K. Richmond

This is a progress report summarizing more than 5 years of a long-range Bureau of Mines research program. The purpose of this program has been to investigate the fire and explosion properties of Green River oil shale in the Bureau's Experimental Mine, in laboratories, and in the field. The lean limits of explosibility of oil shale dust, by small-and large-scale tests, are reported as a function of grade, ignition source, and particle size. A limited number of laboratory tests on the autoignition of oil shale dust layers and the spontaneous combustion tendencies of oil shale are described. Moderate-scale rubble fire tests were conducted to determine flame spread rates as a function of ventilation flow. With the aid of a system to continuously monitor methane emissions in a deep oil shale mine, the characteristics of the methane flow are reported as a function of ventilation and blasting procedures, and are compared with gas yields from core samples. Tentative predictions as to the emission of the methane to be expected in deep oil shale mines, far from the outcrop, are offered. Brief reference is made to a parallel investigation into the fire and explosion hazards of oil shale mining and processing by a Bureau contractor; detailed results of the latter investigation are to be found in the contractor's reports.

Jan 1, 1982

By Siavoljub D. Maksimovic

The Bureau of Mines, through a cooperative agreement with Duquesne Light Co. of Pennsylvania, field tested a method of using pneumatic stowing of crushed limestone to construct seals in long-abandoned mine openings that were part of an active mine closed shortly before sealing. A total of 13 openings at 11 sites were backfilled. In pneumatic stowing, material is conveyed through a pipeline and into the mine opening under low air pressure. The stowing equipment consists of a power sup-ply, a blower, a feeder to inject material into the pipeline, and a nozzle for directing the placement. Material is ejected from the nozzle at high velocity, creating a high-compaction fill upon impact. The fill material used was well-graded limestone aggregate up to 1-1/2 inches in diameter, with sufficient fines. This fill was modified at five locations by the addition of portland cement, expansive cement, and/or bentonite. The pneumatic stowing method is safer and faster than conventional methods, is cost competitive, and eliminates or reduces the exposure of workers to possible hazards since the nozzle can be kept outside the mine opening. The equipment is mobile, but some modifications in the technique would improve performance. The technique was used at remote locations where other methods could not be used without disturbing the environment.

Jan 1, 1982

By Slavoljub D. Maksimovic

The Bureau of Mines, through a memorandum of agreement with the State of Ohio, tested a method of constructing seals in abandoned mine openings in Ohio by means of pneumatic stowing of crushed limestone and gravel with sand. A total of five openings and one shaft were back-filled. Pneumatic stowing uses compressed air to convey material through a pipeline and into the mine opening. The stowing equipment consists of a power supply, a blower, a feeder to inject the material into the pipeline through an airlock, and a nozzle for directing the placement. Material is ejected from the nozzle at high velocity, creating a high-compaction fill upon impact. Well-graded aggregate up to 2 inches in diameter and having sufficient fines is used as fill. The stowing method is safer and faster than conventional methods, is cost competitive, prevents trespass into abandoned mine openings, and eliminates or reduces the exposure of workers to possible hazards since the discharge nozzle can be kept at the mouth of the opening. The equipment is mobile, and, with some modification, the technique could be widely used for sealing abandoned and active mine openings, even in remote locations and during severe weather conditions.

Jan 1, 1982

By R. H. Lien

The Bureau of Mines has conducted research on a flue gas desulfurization (FGD) process as part of its goal of minimizing the undesirable environmental impacts associated with sulfur dioxide (S02)-bearing waste gases. This FGD process, referred to as the modified citrate process, involves absorption of S02 in a buffered citric acid solution. The absorbed S02 is subsequently stripped from the solution using steam, which regenerates the solution and produces a wet S02 product. This product can be further processed to make sulfuric acid or liquid S02. Economic evaluations showed the process to be expensive when the stripper was operated at or near ambient pressures because of the large amounts of steam required for solution regeneration. Research was directed at reducing steam consumption in the stripper. The effect of stripper pressure on steam consumption was investigated. A process research unit (PRU) was operated with the stripper pressurized in the range of 5 to 150 psig. Test results showed that steam consumption decreased with increased stripper pressure. For example, when operating the PRU stripper at 150 psig, 4.1 grams of steam per gram of S02 was required to remove 90 pct of the S02 from a 1.0-vol-pct-S02 gas. This compares to 7.1 grams of steam per gram of S02 required for 90-pct S02 recovery at 5 psig.

Jan 1, 1982

By Theodore L. Turner

This Bureau of Mines report describes calcination of kaolinitic clay in a direct-fired 2-1/2- by 24-ft rotary kiln at 750° and 775° C. Methods for preparing kaolin feed materials and characterization of calcined products are discussed. Approximately 99 pct of the alumina in a typical eastern Georgia kaolin was soluble in HC1 after calcination at either 750° or 775° C.

Jan 1, 1982