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By H. E. Powell

The smelting of brass and bronze generates a dust composed primarily of zinc oxide, with lesser amounts of other metal oxides, such as copper, lead, and tin. The small quantity of this waste generated by individual smelters and the relatively low unit value of the contained metals, suggests the desirability of reclaiming the metals onsite or at some nearby point. The Bureau of Mines has developed a process that fits these requirements. The technique consists of (1) dissolving zinc and copper from the dust with sulfuric acid, (2) recovery of copper by cementation, (3) recovery of zinc as zinc sulfate crystals, and (4) recovery of lead and tin as a salable residue. Alternatively, zinc may be recovered by electrodeposition. Free acid is recycled and no major pollution problems are generated by the process.

Jan 1, 1972

By I. D. Shah

Thermal decomposition of copper (II) sulfate (CUS04) and copper (II) oxy-sulfate (CuO?CUS04) are important steps in the overall oxidative roasting of covellite (CuS) and chalcocite (Cu2S). Nonisothermal thermogravimetric techniques were used to investigate the decomposition reactions in flowing Na and air. Thermal decomposition of CUS04 and CuO?CUS04 followed "linear" kinetics with an apparent activation energy of 55±2 and 66±3 kcal per mole decomposed, respectively. These apparent activation energies comply with those previously reported when isothermal kinetic techniques were used. The addition of oxygen decreased the rate of decomposition, while small amounts of iron which were admixed with CuO?CUS04 did not have a significant effect. Neither oxygen nor iron had any appreciable effect on the apparent activation energy of the decomposition reaction.

Jan 1, 1972

By Martin H. Stanczyk

Ultrafine grinding of the industrial minerals mica, pyrophyllite, talc, marble, barite, and fluorite was accomplished using the Bureau-developed and patented attrition-grinding process. The materials, representing minerals of diverse physical characteristics, were batch ground in a 10-inch-diameter machine using statistically designed experimental test programs. The tests were made to determine large effects of variables such as feed pulp density, grinding medium size, and quantity of the electrical energy consumed during grinding on product particle size and bulk density. In designing the test programs, it was assumed that there was no interaction between the variables. Relatively coarse commercial flotation concentrates of mica, barite, and fluorspar and mine-run products of pyrophyllite, talc, and marble were readily ground into subsieve size ranges. Considering the great amount of particle size reduction obtained, the electrical energy requirements for grinding were very low. In general, the test results indicated that the best conditions for particle size reduction were approached when grinding with the coarser fraction of sand grinding media, the higher-sand-to-mineral weight ratio, and the higher feed pulp density.

Jan 1, 1972

By P. S. Lewis

Shortage of natural gas is reviving interest in low-Btu fuel gas made by gasifying coal in fixed-bed producers. The Bureau of Mines gasified strongly caking Pittsburgh bed coal over test periods lasting four days in an experimental gas producer located at Morgantown, W. Va, Mechanical stirring throughout the fuel bed was effective for keeping the fuel moving and this stirring made the operation successful; hence, the gas producer was named the stirred-bed producer. Nuclear density gages were applied as control instruments to indicate coal flow and fuel level, and to record the frequency and location of void spaces in the bed, The gas, of nominal 140 to 165 Btu/scf calorific value, could be burned in a boiler for generating steam.

Jan 1, 1972

By James L. Konchesky

Crushed coal, consisting of a wide range of sizes, was effectively blended by recycling it through a bin equipped with a particle distributor. Vertical blending was accomplished by simply recycling the coal; it was not significantly influenced by the horizontal blending that was achieved by the distributor. The method was effective, even though the coal was wet and possessed poor flowing characteristics. Recirculation appears capable of providing uniform blends of solids that can be more efficiently processed. Recirculation also appears useful, preceding packaging operations, to insure for blending of solids into specification products. Continuous measurement of the bulk density of the coal by a gamma ray meter proved to be an effective monitor of vertical blending effectiveness.

Jan 1, 1972

By L. A. Haas

S02 reduction with CO was studied in an integral flow reactor at a nominal flow of 0.5 liter per minute. Reactant gas contained 3 percent SO2, 6 percent CO, and the balance He. SO2 conversion was determined for three different types of catalysts. The first consisted of 16 commercial catalysts used for various chemical syntheses. Only the commercial catalysts which contained transition metals in alumina removed more than 30 percent 80a at temperatures below 510° C. Two other types of catalysts were prepared in the laboratory either by pelletizing equal amounts of powdered alumina and transition metal oxides or by impregnating commercial alumina tablets with transition metal ions. Regardless of preparation techniques, Cr and Fe in alumina were the two best catalysts. The observed results suggest that an intermediate (SCO) is formed by the interaction of surface metal sulfides and carbonyls. Alumina then catalyzes the interaction of SCO with S02 to form the end products (sulfur and carbon dioxide). Over 80 percent S02 was removed at 460° C with 2 grams alumina impregnated with 2.5 percent iron.

Jan 1, 1972

By O. Q. Leone

Composite diaphragms were used in the investigation of electrowinning Ti from TiC14 in a fused LiCl-KCI-TiC'2 electrolyte. Composite diaphragms tested were of two general classes--those consisting of two or more solid materials, and those which contained, in addition, a loose material. An electrowinning cell using a flat diaphragm is described. The maximum current density for these diaphragms was 300 amp per ft2. Lower currents permitted longer operation times. The composite diaphragms gave electrode efficiencies that averaged approximately 60 percent, and the electrowon titanium was of good quality--some Brinell hardnesses were as low as 68.

Jan 1, 1972

By W. H. Eddy

The Bureau of Mines conducted laboratory batch and continuous flotation processing tests on waste granite fines from South Carolina to determine the possibility of recovering high-quality feldspar and glass sand. Three flotation systems were used for removal of the iron-bearing biotite: Two employed an alkaline anionic-cationic circuit and the third employed an acid cationic circuit. Commercial-grade products were obtained when the remaining biotite was magnetically removed from the feldspar and quartz concentrates. Continuous flotation processing yielded a feldspar concentrate containing, in percent, 3.60 Na20, 5.60 K20, and 2.25 Ca0, with recoveries of 75.3, 66.6, and 72.6 percent, respectively. The feldspar tailing was high quality glass sand containing 98.0 percent Si02 and 0.025 percent Fe203; about 60 percent of the quartz was recovered.

Jan 1, 1972

By J. J. Henn

A process is evaluated for recovering metallurgical-grade manganese are from the low-grade manganiferous iron ores of the Cuyuna Range, Minnesota. The process, developed by the Bureau of Mines, employs high-temperature sulfatization of the are to form manganese sulfate and reduction of the are to convert the iron to a magnetic oxide. The roasted ore is water-leached to dissolve the manganese sulfate, which is then separated from the leach residue, is crystallized, and is calcined to produce the manganese product. Iron is recovered from the leach residue by magnetic separation, and is pelletized and calcined to produce byproduct iron ore pellets. The fixed capital cost for a plant yielding a product containing 100 tons of manganese per day is $19.6 million on a mid-1970 basis when the raw are contains 4.84 percent manganese. The estimated operating cost of the plant is $211 per ton of contained manganese. Graphs are included to show the effects of ore cost and varying manganese content of the raw ore on the estimated operating cost.

Jan 1, 1972

By John P. Gooch

The solubility of 1,1,2,2-tetrabromoethane (TBE) in water was determined from 1.0° to 97.0° C. The solubility (S) of TBE in grams of solute per 100 grams water was correlated with [S = 1,920.55 [exp (40292L7 11, T2 10 T 737.577 + 9.923962 ] where T is in degrees Kelvin. A thermodynamic analysis conducted on a system consisting of a TBE phase and a water phase in equilibrium with a vapor phase led to the calculation of the activity coefficient, vapor-liquid equilibrium distribution coefficient, relative volatility, and heat of mixing for saturated solutions of TBE in water. Data required for these calculations were the solubility of TBE in water and the vapor pressures of TBE and water as a function of temperature.

Jan 1, 1972

By M. G. Zabetakis, T. D. Moore

The use of a partially slotted 6.5-inch-inside-diameter vertical pipe to remove methane from a longwall gob area at a depth of 2,260 feet in the Pocahontas No. 3 coalbed ms investigated. The value of gas removed by such a pipe under free-flow conditions was found to equal the cost of the installation in this case. Approximately 25 percent of the available methane passed through the pipe without the use of an exhauster; an additional 10 percent was removed when an exhauster was employed. The diversion of methane through a vertical slotted pipe to the surface permitted the use of increased mining rates and decreased the ventilation air requirements.

Jan 1, 1972

By T. D. Moore

The use of a partially slotted 6.5-inch-inside-diameter vertical pipe to remove methane from a longwall gob area at a depth of 2,260 feet in the Pocahontas No. 3 coalbed was investigated. The value of gas removed by such a pipe under free-flow conditions was found to equal the cost of the installation in this case. Approximately 25 percent of the available methane passed through the pipe without the use of an exhauster; an additional 10 percent was removed when an exhauster was employed. The diversion of methane through a vertical slotted pipe to the surface permitted the use of increased mining rates and decreased the ventilation air requirements.

Jan 1, 1972

By A. E. Nagel, J. E. Carpetta, M. G. Zabetakis, T. D. Moore

The method of moving averages was found useful in assessing the nature of methane emission in coal mines. Emission rates were influenced markedly by the presence of abandoned oil and gas wells in the vicinity of the mine. Such wells appeared to increase the flow rate of methane into the mine by a factor of 2 to 30 in an active mine in the Pittsburgh coal seam.

Jan 1, 1972

By Foster Fraas

A comparison has been made between cubes and spheres in the matrix of the high-intensity wet magnetic separator. For two inclined plane surfaces, such as may occur with cubes, the maximum force value, H [dH-dx] is at the point of nearest approach and is much higher than the force resulting from adjacent spheres. Although the maximum force value for cubes is higher, it decreases more rapidly at increasing distances. The maximum force for spheres is at an appreciable distance from the point of nearest approach. At field intensities for magnetic saturation of the iron spheres, the force extends to further distances with greater uniformity approximating that of the constant force or isodynamic field. The force is also independent of the sphere diameter, which permits the scaling of the sphere diameter to provide changes in particle migration distances without changes in force gradient.

Jan 1, 1972

By H. E. Powell

A solvent extraction procedure was developed on a laboratory scale for recovering trisodium phosphate, zinc, and iron from waste phosphate sludge as separate products. The sludge was dissolved in hydrochloric acid, and iron was extracted as ferric chloride by isopropyl ether. Zinc was extracted by di-2-ethylhexyl phosphoric acid in kerosine. The efficiencies of the one-and two-stage extractions ranged from 98 to nearly 100 percent. Trisodium phosphate was recovered by crystallization from the raffinate. The value of two marketable products is considerably more than than the costs of the major reagent. The process was developed to permit recycling of values in this waste and to consequently reduce stream pollution from this source.

Jan 1, 1972

By D. J. Bauer

A solvent-extraction system employing selective stripping of a pre loaded organic phase was investigated for recovering Sm203 from a light-group rare-earth mixture. The samarium concentrated in the organic phase, and a >99-pct-pure samarium oxide product was obtained at 76-pct recovery in a 20-stage operation using di(2-ethylhexyl) phosphoric acid (EHPA) as the organic phase. The stripping agent was a 1.5-pct hydrochloric acid solution containing 200 g NH4C1/1.

Jan 1, 1972

By Richard J. Kline

The underground mining industry is presently using the fluid network analyzer and digital computer to analyze ventilation systems. The availability of the digital computer and ventilation programs to mining companies has escalated its use, permitting the design and modification of new or existing mine ventilation systems to be projected completely and thoroughly with consistent precision. Because the analog computer has been analyzing ventilation systems accurately for many years, a comparison of the analog and digital methods was warranted. This report summarizes a detailed comparison for one mine, based on parallel analyses by the two computer systems.

Jan 1, 1972

By R. V. Higgins

A numerical method is presented to calculate the pressure distribution in a petroleum reservoir that has irregular boundaries. The computer program is straightforward and requires minimal data preparation. The method can also be used to determine pressure distribution in many other types of underground reservoirs. In this method, the grid solution of the fluid-flow equations in a reservoir that has regular boundaries (previously published) was expanded to handle irregular boundaries. The computer program locates grid points at the irregular boundaries. The method of mirror images is then used to form a special stencil to determine the pressure at each of these points. Two examples are presented to demonstrate the applicability of the method for virtually any reservoir configuration.

Jan 1, 1972

By K. R. Becker

The addition of a force gage and a reaction detector to the Bureau of Mines drop-weight impact apparatus made it possible to examine the details of the force exerted on the specimen and make estimates of the time to reaction. With the current setup the force was found to be oscillatory and not reproducble. However, single well-defined pressure pulses can be delivered to the explosive sample by modifying the drop-weight tools. With a modified test arrangement, the time to reaction and the peak force and energy at the time of reaction were determined as a function of drop-weight height for several different explosives. All these parameters were found to decrease as the rate of force application was increased. The same parameters were also found to vary with the thickness of the test sample. The implications of these results are discussed in terms of practical drop-weight testing.

Jan 1, 1972

By C. C. Merrill

Columbium, tantalum, titanium, and zirconium are present in solid waste products generated by the chlorination of rutile used for production of titanium tetrachloride (TiC14). The columbium and tantalum were separated from titanium and zirconium by liquid-liquid extraction techniques using a secondary amine. Salts of these elements are in a leach liquor produced by water leaching of mineral waste from the chlorination of rutile. This waste, produced at the rate of approximately 50,000 tons per year, is about 40 wt pct water soluble. Leach liquors, separated by filtration, were further separated into a solid fraction and a liquid fraction by pressure hydrolysis, The solid fraction containing Cb, Ta, Ti, and Zr was dissolved in HC1-HF and used as a feed solution. Columbium and tantalum were removed from the organic extractant with 1 [N] HC1. A miniature 10-stage reactor showed that the columbium and tantalum present in solution could be separated with a continuous flow.

Jan 1, 1972