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By D. D. Fischer

Recovery and separation of molybdenum and rhenium from a process solution was accomplished by a technique developed by the Federal Bureau of Mines involving a combined solvent extraction and activated carbon adsorption procedure. The processing sequence required treatment of the solution with S02 to reduce the chlorate ion and adjust the pR prior to solvent extraction of molybdenum and rhenium with a tertiary amine. Molybdenum and rhenium were stripped from the organic phase with an NH40H solution, and the strip solution was then passed through activated carbon to preferentially adsorb the rhenium. After washing entrained molybdenum from the column with a brine solution, rhenium was eluted with an MeOH-H20 mixture. The activated carbon was regenerated with water. Molybdenum was recovered as (NH4)6Mo7024 by evaporating the column effluent. Rhenium in the column eluate was reextracted with a tertiary amine, stripped from the organic phase with dilute NH40H, and recovered as NH4Re04 by evaporating the strip solution. The final (NR4)Re04 product contained < 80 ppm impurities. Sodium sulfate was crystallized from the first solvent-extraction raffinate by lowering the solution temperature to 0° C. Precious metals contained in the original process solution were adsorbed onto the activated carbon.

Jan 1, 1975

By W. E. Lamont

The Federal Bureau of Mines, in cooperation with phosphate companies in the Florida land-pebble area, made a comprehensive study of the waste clays, or "phosphate slimes," produced in the mining of phosphate rock in Florida. These slimes represent a significant ecological problem and a major deterrent to effective land recovery in the phosphate-mining areas. Physical, chemical, and mineralogical studies were made of slime samples submitted by 15 of the 16 plants in Florida in an effort to identify factors that prevent successful consolidation of the slimes and subsequent recovery of the mined lands. Results of these studies indicated that the clay mineral attapulgite, a hydrated magnesium silicate, was primarily responsible for the very poor settling characteristics of the slimes, and that the quantity of attapulgite in the slimes effectively controlled the settling rate, pulp density of terminal solids, viscosity, percent solids of filter cake, and flocculant requirements.

Jan 1, 1975

By J. R. Cobble

The Federal Bureau of Mines conducted static tests at 2,500° F on 39 refractory compositions, and dynamic tests at [2,825°35° F] on 31 commercial refractory brick specimens to determine their resistance to corrosion and erosion by a slag similar in composition to that used in producing insulating mineral wool. The static tests showed fireclay, low-alumina compositions (<70 percent A1203), zircon, zirconia, SiC, and clay-bonded graphite refractories to be unsuitable. Dynamic test results indicated that magnesia and chromia compositions were superior to high-alumina compositions (=70 percent A1203) as a furnace lining for melting mineral wool. Data from these tests indicated that magnesia and chromia compositions with low RO/R203 mole ratios were more resis tant to attack by mineral wool slags than ones with high RO/R203 mole ratios.

Jan 1, 1975

By B. J. Scheiner

The Federal Bureau of Mines investigated an electrolytic oxidation procedure for extracting lead, zinc, copper, and silver from lead-zinc concentrates. Concentrates slurried in brine were pumped through the anode compartment of electrolytic cells equipped with selective ion diaphragms. Hydrochloric and hypochlorous acids generated in the anode compartment converted the metal sulfides in the concentrates to soluble metal chlorides, sulfate ion, and elemental sulfur. Metal extractions of 92 to 100 pct were obtained from lead-zinc concentrates at an energy consumption ranging from 1.5 to 5.0 kW-hr/lb metal extracted. Sodium hydroxide was formed in the cathode compartment at a current efficiency of >99 pet. Silver and copper were extracted from refractory tetrahedrite minerals, but the process entailed a relatively high energy consumption. Sealing the top of the diaphragm cell utilized the chlorine more effectively, thereby reducing energy consumption 10 to 50 pct.

Jan 1, 1975

By W. P. Diamond, B. M. Bench, C. M. McCulloch, Maurice Deul

As part of the Bureau of Mines methane control program, the Pittsburgh coalbed was studied in Washington and Green Counties, Pa., and in Marion and Monongalia Counties, W. Va., where this coalbed is now being mined at its greatest depth. The coalbed thickness appeared to be structurally controlled; the bed was generally thinner near the axes of anticlines and thicker near the axes of synclines. The overburden isopach shows a similar relationship. Most of the clay veins in coal occur in the synclinal troughs, generally under sandstone roof. Cleat orientations measured in 18 underground mines showed that face cleats are perpendicular to the axial trends of the folds, and the butt cleats are parallel to the axial trends, indicating structural control of the cleat. Measurement and analysis of surface joint orientations provide a method for predicting the cleat orientations of the coalbed, but linears measured from infrared photographs and photoindex sheets helped only to determine regional trends. The results of these investigations provide a geologic framework for rational planning for underground mine development to use the best available technology to cope with methane emissions, coalbed discontinuities, and related ground support problems.

Jan 1, 1975

By George A. Savanick

An experimental hydraulic jetting device intended to operate in a 16-in-diam borehole was designed, fabricated, and used to cut coal and simulated coal samples. This device consisted of two 0.107-in-diam nozzles that rotated in a plane perpendicuIar to a 50-inch length of high-pressure tubing. Experi¬ments were also conducted with stationary jets issuing from a single 0.142-in-diam nozzle. Numerous experiments were performed using systematic variations of jet parameters coupled with assessments of cutting rates. These Bureau of Mines tests showed that when operated at 4,000 psi pressure and a 40-gpm flow rate (1) the device can fragment coal up to a distance of 8 feet from the nozzle, (2) 4,000-psi jets cut more effectively than lower pressure jets with the same nozzle diameter, (3) stationary jets do not cut as effectively as moving jets, (4) interkerf breaking occurs when the kerf spacing is less than 2 inches, and (5) if the kerfs are spaced <1/2 inch, the jet is deflected and thereby reduces cutting effectiveness.

Jan 1, 1975

By S. R. Borrowman

Mill tailings from conventional uranium extraction processes contain nearly all of the radium originally in the ore. Such tailings require controlled storage in perpetuity to safeguard the surrounding environment from radioactive contamination. Alternatives to controlled storage of the tailings are (1) removal of the radium from the tailings for separate storage or use or (2) removal of the radium when processing the uranium ore. In laboratory tests conducted by the Federal Bureau of Mines, radium was leached from tailings using either hydrochloric acid or ethylenediamine tetraacetic acid. A hydrochloric acid leaching method was used to extract both radium and uranium from the ore to yield tailings containing less radium than those produced by either conventional sulfuric acid or alkaline leaching processes. From 77 to 94 percent of the radium in mill tailings was concentrated by sedimentation in slime fractions representing nearly 25 weight-percent of the original sample.

Jan 1, 1975

By J. C. Franklin

A data-acquisition system was designed by the Bureau of Mines to monitor five detectors with radon continuously flowing through each. These detectors could be monitored up to 12 times an hour, but were only monitored according to a preset time, thus allowing radon to be monitored continuously in a uranium mine. The counter can be set to monitor each detector for any period of time up to 16.5 minutes. This allows very low concentrations to be monitored longer to reduce statistical error. There would be no upper limit in radon concentration that could be monitored, but there would be a lower limit of 50 picocuries per liter (pCi/l). Each detector was cylibrated in the laboratory by the Lucas flask method. Multiple samples were taken at two different concentrations, and the correction factor for each detector was determined by a least squares fit of the data. To verify the calibrations, a series of measurements at several concentrations were made against a constant source. Our agreement at low radon concentrations (300 pCi/i) with the two-filter method as within 3 percent; thus, the total error would be this difference plus the two-filter error. At high concentrations the coefficient of variation ranged between 2.1 and 9.8 percent for the five different detector units.

Jan 1, 1976

By R. A. Guidotti

The Federal Bureau of Mines studied the thermal decomposition of the nitrides of the Group V A metals (CbN, Ta3N5, and VN) with the goal of preparing high-purity metals. Solid-state purification and arc and electron-beam melting were examined. Electron-beam melting proved to be the most efficient means of nitrogen and oxygen removal. Columbium and tantalum of 99.9-pct purity were prepared by this technique; in the case of vanadium, however, nitrogen could not be reduced below the solid-solution level.

Jan 1, 1976

By K. J. Liles

Research was undertaken by the Bureau of Mines to determine the technical feasibility of producing lightweight aggregate from the waste glass fraction of municipal incinerator residues. Tests were conducted to determine the amount and optimum size of glass, the amount of sodium silicate, and the method used to form the material to be expanded. The most suitable mixture, 78 percent glass, 20 percent clay, and 2 percent sodium silicate, was pelletized and then expanded by exposure to a temperature of 1,550° F for 15 minutes The resulting lightweight material had a bulk density of 38 lb/cu ft and exhibited excellent pore structure. Concrete test cylinders made from the light weight aggregate had a unit weight of 104 lb/cu ft and a compressive strength of 2,550 lb/sq in after a 28-day steam cure.

Jan 1, 1976

By F. P. Haver

Primary lead is produced in the United States by the pyrometallurgical smelting of lead sulfide (galena, PbS) concentrates, which poses sulfur dioxide and lead air pollution control problems. The Federal Bureau of Mines has investigated an alternative hydrometallurgy procedure that does not generate gaseous sulfur oxides and diminishes the potential for the escape of lead into the atmosphere. The procedure involves leaching galena flotation concentrates with ferric chloride (FeC13) solution to obtain lead chloride (PbC12) and elemental sulfur as expressed by the following chemical reaction: PbS + 2FeC13 ? PbC12 + 2FeCl2 + S°. At 100° C, over 99 pct of the PbS in the concentrate is converted to PbCl2 in less than 15 min. The leach solution, composed of brine (NaCl) containing slightly more than the theoretical required amount of FeC13, dissolves the PbC12 as it is formed, leaving a residue of elemental sulfur plus gangue. High-purity PbC12 (>99.9 pct) crystallizes from the leach filtrate on cooling and is electrolyzed in a low-temperature, fused-salt cell to obtain corroding-grade metal (>99.94 pct Pb). Spent leach solution (FeC12) is regenerated for further use by reaction with the chlorine obtained in the electrolysis of lead chloride. Other values, such as Ag, Cu, Zn, and S°, are recovered by additional treatment of either the leach solution or leach residue.

Jan 1, 1976

By Carl F. Wingquist

Electrical resistance heating to effect thermal fragmentation of semiconductive rock was examined by the Bureau of Mines. Tests were carried out on copper-bearing ores of the Nonesuch Shale Formation in the laboratory and in the the field at White Pine, Mich. Fieldwork included primary and secondary breakage tests. Heating tests on in situ rock failed to produce thermal dam-age to an extent considered useful; however, boulders up to 30 ft3 were effectively broken by the method. Power input to the test rock was taken from a 50-kV, 5-amp dc power supply.

Jan 1, 1976

By Arthur M. Hartstein

The Federal Bureau of Mines, under a contract with Ultrasystems, Inc., investigated the thermal oxidative degradation characteristics of conveyor belts used in underground mines. This included the determination of smoke evolution, glow characteristics, char yields, and the identification and quantification of all volatile decomposition products in the form of gram of specific product formed per gram of belt sample tested. In addition to these investigations, degradation studies were conducted on some pure ingredients used in conveyor-belt formulations. Three basic classes of belts were investigated: neoprene, polyvinyl chloride, and styrene-butadiene rubber compositions. The studies indicate that styrene-butadiene-based belts exhibit good flame resistance and are the least hazardous in regard to overall formation of toxic decomposition products. Under this program, thermogravimetric analysis was definitely established as a method of material differentiation.

Jan 1, 1976

By E. E. Maust

The literature on the activation of sphalerite for flotation by short¬chain xanthates leaves unanswered the question of whether a compact surface film of activator sulfide is necessary or merely sufficient for high flotation recoveries. Studies by Guarnaschelli and Plaksin indicate that xanthate adsorption and flotation of sphalerite are increased with increasing hole/ electron ratio. These results, and the known acceptorlike behavior of many heavy-metal impurities in zinc sulfide, suggest that activation may result from a traditional semiconductor doping effect at the surface. Using the theory of chemisorption states on ionic crystals as developed by Levine and Mark, the Bureau of Mines has carried out A calculation to estimate the surface-state energies of various metals when they are substituted at zinc sites on (110) sphalerite surfaces. Based on a simple Madelung-Born treatment of ionic solids, the calculation indicates that many of the metals known to activate sphalerite for subsequent flotation have lower surface-state energies than nonactivators. The results of these calculations are discussed from the standpoint of consistency with the proposed activation mechanism and observed flotation results. The satisfactory agreement obtained is taken to be support for the proposed mechanism, and further elaboration of a surface-doping model is attempted.

Jan 1, 1976

By Joan T. May

The Bureau of Mines conducted laboratory tests to evaluate the production of high-purity H3P04 by HCl digestion and solvent extraction. Both batch and bench-scale continuous tests were made. Western phosphate rock concentrates were acidulated with HCI, and the digestion liquors were processed by solvent extraction. Phosphoric acid was extracted with isoamyl alcohol and recovered from the organic extract by contact with an NH4F solution. This solution was fractionally distilled to yield high-purity H3P04. The raffinate from solvent extraction was treated with lime to precipitate CaF2, which was subjected to steam pyrolysis to generate HF. This method was successful in recovering 95 pet of the phosphate and 80 pct of the fluoride contained in the concentrates.

Jan 1, 1976

By K. C. Dean

Time and motion studies were made by the Federal Bureau of Mines on the hand and machine dismantling of scrapped auto starter motors, generators, and alternators for recovery of copper, aluminum, and iron. The studies showed that an individual with power handtools and convenient access to a hydraulic press, power bandsaw, acetylene torch, and power lathe could, in an 8-hour day, disassemble about 100 starters, or 150 generators, or 30 alternators. The scrap copper yield would be 280, 390, and 45 pounds, respectively, and the iron yield would be about seven times the copper weight. About 100 pounds of aluminum would be obtained from the alternators.

Jan 1, 1976

By L. W. Higley

Electrowinning metals from solutions leached from low-grade ores is becoming an increasingly important extraction method as the metal industry turns to pollution-free recovery processes. Lead-alloy anodes are used industrially in the electrolytic recovery of zinc and copper. However, associated with the use of these anodes are the inherent problems of stability and lead contamination of the cathode. In an effort to eliminate these problems, the Bureau of Mines has developed a relatively inexpensive lead dioxide anode for electrowinning metals from strong acid solutions. The anode was prepared by depositing Pb02 directly on a titanium blank in a strong HN03-Pb(N03)2 solution at 2.15 to 6.45 A/dm2 and 60° C. This anode was tested in zinc and copper electrowinning cells containing 200 gpl H2S04 and 35 to 100 gpl metal ions at the current density of 3.23 to 6.45 A/dm2. Contamination of the cathode by lead was =0.005 pet. A 30-day test at 6.45 to 12.90 A/dm2 in an electrolyte containing 200 gpl H2S04 and no metal ions resulted in a slight change in surface morphology of the Pb02 anode but no measurable change in anode weight or dimensions.

Jan 1, 1976

By Noel N. Moebs

Valley Camp No. 3 mine was the scene of an experimental shortwall introduced in 1973 in an attempt to improve the recovery from the Pittsburgh coalbed in the Ohio Valley area where adverse ground conditions have imposed partial extraction methods with only 40 to 55 percent recovery of the valuable resource. The Bureau of Mines, under a cooperative agreement with Valley Camp Coal Co., monitored ground pressures and caving in the shortwall section in an effort to determine whether the roof strata, notably the limestone main roof, will cave to the extent that roof pressures at the face are relieved and whether the powered roof supports can sustain the roof load. The Bureau&apos;s efforts included mapping of clay veins, instrumentation of chain pillars and shortwall panels with encapsulated pressure cells, recording hydraulic pressures in the legs of the shortwall chocks, and core drilling underground and from the :surface. The experimental shortwall was a qualified success. Recovery increased 5.4 percent compared with partial extraction. Pressures in chain pillars and the abutment zone were not excessive. Hydraulic pressures in the chock legs did not approach the yielding pressure. Apparently, the limestone strata caved and the roof pressure at the face was relieved.

Jan 1, 1976

By Philip E. Sanker

The Bureau of Mines conducted small-scale batch and semicontinuous tests on the reduction of zinc sulfide with iron according to the reaction ZnS + Fe ? FeS + Zn to determine reaction kinetics in the temperature range 1,000° to 1,400° C and to investigate the potential use of a scrap iron reductant. Batch tests indicated that a temperature of at least 1,300° C with a 1:1 mole ratio of Fe to ZnS is needed for good zinc recovery. Semicontinuous tests were conducted, using four zinc concentrate samples, containing various percentages of copper, cadmium, and lead, which were reacted with iron and iron contaminated with iron oxide and tin in an externally heated graphite furnace. Analysis of the zinc metal and FeS matte reaction products showed cadmium to be entirely in the zinc metal, copper to be in the FeS matte, and lead to be about 60 pct in the zinc metal and 40 pct in the matte. Tin reported to the matte, and none was detected above the O.OS-pct level in the zinc. Sulfur dioxide was not detected in the offgas when up to 20 pct of the iron was replaced by Fe203.

Jan 1, 1976

By J. R. White, S. W. Lambert, C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08" for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976