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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 G. B. Atkinson

To develop technology to help assure an ample domestic supply of zinc, the Bureau of Mines is investigating an aqueous chlorine-oxygen leaching process for treating complex sulfide concentrates. This report discusses the purification of aqueous C12-02 leaching solutions by utilizing zinc cementation to remove Cd, Co, Cu, Ni, and Pb. Additional processing of the purified solution is necessary to produce ZnC12 crystals suitable for molten-salt zinc electrowinning cells. The effects of solution temperature, reaction time, zinc dust concentration, ZnCl2 concentration, and degree of agitation on the removal of impurities were investigated for both simulated and actual leaching solutions. Zinc dust addition to a leaching solution at 30° C decreased the Cd, Cu, Ni, and Pb concentrations to acceptable levels of less than 3 mg/1 each. By increasing the solution temperature to 75° C, the cobalt content was decreased to less than 5 mg/l, an acceptable level for producing electrolytic cell-grade ZnC12. Impurity removal rates from ZnCl2 solutions are Pb>Cu=Cd>Ni>>Co. An increase in the solution temperature increases the rate of removal for these metal impurities.

Jan 1, 1982

By Martin Hertzberg

The Bureau of Mines 8-liter flammability system was used to study the effectiveness of a variety of powdered inhibitors in preventing the propagation of explosions of coal dust or methane in air. Over 35 different chemical additives were evaluated against Pittsburgh seam pulverized coal. The least effective inhibitors were the carbonates, which required mass additions in the range of two to three parts inhibitor to one part of coal dust in order to prevent propagation. The most effective inhibitors were the derivatives of ammonium phosphate, which were effective quenching agents at additions of only one part inhibitor to four parts of coal dust. Alkali halide powders were of intermediate effectiveness. These laboratory-scale results are in good agreement with full-scale mine experiments in all cases where detailed comparisons have been made. Data were also obtained for the effectiveness of several of the same powdered inhibitors against methane-air explosions. Their relative order of effectiveness and the concentration ranges required for quenching the gas explosion are comparable to those measured for coal dust explosions. Data are also presented for the effectiveness of N2 and CF3Br addition. Some preliminary data are also presented for powder addition to methane burner flames. Those data are compared with other burner data and evaluated in terms of their relevance to explosion tests.

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 J. M. Stuve

A novel calorimetric solution technique, recently developed at the Bureau of Mines, was tested using synthetic samples of chalcocite (CU2S) and covellite (CuS). The solution of these refractory sulfides was accomplished by oxidation with bromine in a moderately acidic, aqueous solution. The resulting values for the standard enthalpies of formation (?Hf°, 298.15) for CU2S(c) and CuS(c) were -18.1 ±1.1 kcal/mol and -13.3 ±1.1 kcal/mol, respectively. These values are in good agreement with published formation values derived from other methods of physicochemical measurement.

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 D. J. MacDonald

The Bureau of Mines has carried out investigations on a method for producing zirconyl sulfate solution from zircon sand, comprising (1) reacting zircon sand with molten NaOH, (2) leaching the resultant fusion frit with water to remove sodium silicate and to convert sodium zircon-ate to hydrous zirconium oxide, and (3) leaching the hydrous zirconium oxide from unreacted sand with hot, dilute H2S04 to produce crude zirconyl sulfate solution. The following conditions were found to be suitable: reacting 0.6 kg of NaOH per kilogram of zircon sand for 10 min at 600° C; leaching the frit with 3 to 4 liters of water per kilogram of solids; leaching the residue with 5.1 liters of water and 1.25 liters of 98-pct H2S04 per kilogram of original solids for 10 min at 90° C; and filtering or decanting to recover unreacted zircon sand. A preliminary cost estimate is included.

Jan 1, 1982

By Kenneth O. Bennington

This investigation is part of the Bureau of Mines research effort directed at advancing mineral technology and minimizing energy requirements for extractive metallurgy. The emplacement of the primary minerals petalite (LiAlSi4010) and spodumene (LiAlSi206) in the lithium pegmatites is examined on the basis of their Gibbs energies of formation determined from lithium metastltcate and oxides, using a series of proposed reactions. The reaction between spodumene, quartz, and petalite (LiAlSi206 + 25i02 [=] LiAlSi4010) apparently does not take place in nature but may be proved experimentally.

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 Robert C. Gabler

The extraction of metals from coal ash was investigated by the Bureau of Mines in an effort to produce a more environmentally acceptable waste and offset waste disposal costs with recovered metal values. The research was conducted in two steps: determination of the parameters that affect extraction of metals from coal ash and development of extraction-recovery procedures. Data obtained indicate that the major parameter affecting the extraction of metals from coal ash is the calcium content of the ash. Other parameters such as furnace type and operating temperature had much smaller effects on metal extraction. Two procedures were studied for metal extraction: an acid leach procedure for high-calcium ashes and a lime sinter-acid leach procedure for low-calcium ashes. An alumina product was recovered that, with sufficient washing, meets Hall cell specifications. The leach residues pass the EPA EP Toxicity Test and are thus nonhazardous wastes available for a variety of uses.

Jan 1, 1983

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 T. M. Kohler, G. L. Finfinger, D. M. Hyman, A. T. Iannacchione

The Bureau of Mines measured methane emission rates from an advancing salt face ranging from 15 to 56 ft3/ton (0.5 to 1.8 m3/t). Small room size, use of a continuous miner, and a well-defined ventilation system made possible air velocity and methane concentration measurements, These measurements, representing data from 18 production days, were con- ducted in an area of abnormally low grade salt, Methane emissions occurred primarily during the advance of the salt face by continuous miner.

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