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By Mark I. Copeland

The Bureau of Mines discovered that silicon and nickel additions can prevent the formation of copper alloys of Sn, Sb, and As on the surface of steel during reheating to hot-working temperatures. When molten, these copper alloys cause surface hot shortness during hot working. Wrought steels were reheated isothermally and by simulated industrial practice; the resulting surfaces were metallographically evaluated. The steels contained, In weight-percent, 0.20 C, 0.45 Mn, and up to 1.00 Si, 1.00 Cu, and 0.15 Ni, and up to 0.30 Sn, Sb, or As. The larger the Cu, Sn, Sb and As content of the steels, the greater the amount of silicon necessary to prevent copper alloy formation. A content of 0.10 Ni considerably decreased the amount of silicon necessary for copper steels containing tin and antimony, but not for those containing arsenic. Theories for the beneficial effect of silicon and nickel additions are presented.

Jan 1, 1975

By E. S. Shedd

Amenability studies were conducted by the Federal Bureau of Mines on an electrooxidation technique for the extraction of mercury from cinnabar ores, particularly those that are too low in grade to be furnaced or retorted economically. Oxidation was accomplished by electrolysis of the ore while slurried with brine. Mercury was dissolved through the formation of the soluble tetrachloro mercury complex, HgC142-. Mercury extractions ranged from 90 to 98 percent in 4 to 6 hours of processing time when tests were made on eight different types of cinnabar ores containing from 0.7 to 18 pounds mercury per ton ore. Salt concentration was varied from 4 to 10 weight-percent depending on whether Pb02 anodes and iron cathodes were used or whether graphite was used for both electrodes. Power consumption ranged from 17 to 64 kilowatt-hours per ton of ore treated. Ninety-nine percent of the mercury was recovered from pregnant solutions by precipitation on an active metal such as zinc, followed by distillation of the resulting amalgam at 600° C.

Jan 1, 1975

By T. A. Sullivan

The use of sulfur combined with either sand or waste copper tailings was investigated by the Bureau of Mines as a substitute for a good graded aggregate in asphalt paving materials. The research was part of a utilization program to develop meaningful uses for a projected oversupply of sulfur. Many sections of the country lack good aggregate for paving but do have available sources of sands and sulfur. The development of paving mixtures of desert sands or tailings with sulfur and asphalt was accomplished in the laboratory and tested by laying small paving test sections. Three types of material were studied for use with the sulfur and asphalt. They were (1) a concrete sand similar in gradation to river or beach sands, (2) desert blow sand, and (3) waste copper tailings. Desert blow sand and waste copper tailings are much finer than concrete sand. Mix designs were established for the three types of materials, sulfur, and asphalt used in the paving materials. The best mix designs were as follows, in weight-percent: 80.5 concrete sand, 13.5 sulfur, and 6 asphalt; and 77 either blow sand or tailings, 17 sulfur, and 6 asphalt. Small-scale testing showed that these mixtures were suitable paving materials but would require specialized equipment for transporting and laying. The chemical modification of sulfur to obtain properties that would allow placement of these materials with normal asphalt paving equipment was studied. Results indicate that reacting sulfur with dicyclopentadiene before adding it to the paving mixture was effective in modifying the sand-sulfur-asphalt paving so it could be placed and rolled with conventional equipment.

Jan 1, 1975

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 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 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 H. H. Fields, Joseph Cervik, G. N. Aul

Coal is a soft and brittle material. Drilling rates in the Pittsburgh coalbed using a drag bit exceed 3 ft/min at 2,500-pound thrust. However, maintaining the bit on a horizontal trajectory or parallel to bedding planes to attain lengths of 1,000 feet is difficult. This Bureau of Mines report presents a drill string configuration that can be guided through the coalbed. The angle of the borehole is measured periodically and by proper combinations of bit thrust and rotational speed (r/min), bit trajectory can be lifted or dropped to keep the bit in the coalbed. An example of a hole drilled to 2,126 feet is presented to show levels of thrust and rotational speed used to lift or drop the bit, the seemingly unexplainable events that occur, and the strategy used during drilling. Thrust levels during drilling range from 600 to 2,500 pounds. Hydraulic motors powered by a 30-hp, 440-volt motor provide ample power for drilling horizontal holes 2,000 feet long.

Jan 1, 1975

By Joseph Cervik

Coal is a soft and brittle material. Drilling rates in the Pittsburgh coalbed using a drag bit exceed 3 ft/min at 2,500-pound thrust. However, maintaining the bit on a horizontal trajectory or parallel to bedding planes to attain lengths of 1,000 feet is difficult. This Bureau of Mines report presents a drill string configuration that can be guided through the coalbed. The angle of the borehole is measured periodically and by proper combinations of bit thrust and rotational speed (r/min), bit trajectory can be lifted or dropped to keep the bit in the coalbed. An example of a hole drilled to 2,126 feet is presented to show levels of thrust and rotational speed used to lift or drop the bit, the seemingly unexplainable events that occur, and the strategy used during drilling. Thrust levels during drilling range from 600 to 2,500 pounds. Hydraulic motors powered by a 30-hp, 440-volt motor provide ample power for drilling horizontal holes 2,000 feet long.

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 B. T. Brady

Laboratory measurements by the Bureau of Mines indicate that failure in dry rock specimens measuring approximately 13 cm in length is preceded by tilt anomalies lasting a few milliseconds. The tilt behavior is qualitatively similar to that reported to precede earthquakes. Test results suggest that the time duration of this tilt anomaly for laboratory specimens of this length is independent of rock type, in agreement with theoretical predictions and other experimental data on rock failures including earthquakes.

Jan 1, 1975

By R. L. Stein

For the past several years, the Bureau of Mines has been actively engaged in developing two new oxygen self-rescuers through research contracts with private industry. These new oxygen self-rescuers are designed to be carried by a miner while he is at work and are used during emergency escape, supplying high-purity oxygen to the user and, at the same time, absorbing carbon dioxide (C02), The first of the two new self-rescue breathing devices is a 10-minute, self-contained apparatus developed by the Mine Safety Appliance Co, Size and weight of the unit are comparable to the currently used self-rescue devices. The second device, designed and developed by Lockheed Missiles and Space Corp., is 8. 4.5-lb package which supplies 1 hour of oxygen to the miner. Both devices have a canister which contains the oxygen-producing and CO2-absorbing potassium superoxide chemical, a breathing bag, a bite-type mouthpiece, noseclip, goggles, and hoses connecting the canister and mouthpiece. When needed in an emergency, the miner removes the outer protective cover and dons the unit. For both devices oxygen is immediately available once the mouthpiece is placed in the mouth. These two new units have received prototype approval from the National Institute for Occupation and Safety Health (NIOSH) and the Mining Enforcement and Safety Administration (MESA).

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 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 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 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 P. T. Brooks

Electrochemical machining sludge, a troublesome fluid waste product, was dewatered on a bench-scale basis by three alternative methods tested by the Federal Bureau of Mines. These methods would enable recycling 89 percent or more of the liquid content of the sludge and allow the dewatered solids to be dumped as landfill or processed further to recover contained nickel. Dewatering by vacuum precoat filtration was estimated to be the least expensive. Based on treating 20,000 gallons per day of sludge, precoat filtration costs were estimated as totaling 1.96 cents per gallon of sludge. Two options of an alternative method, comprised of acidification, reprecipitation, thickening, and filtration, were estimated to cost either 3.41 or 3.60 cents per gallon of sludge.

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. B. Janus

This report, the 25th in a series, lists analytical data of coal samples collected by the Bureau of Mines in connection with the purchase of several million tons of coal for various Government agencies during fiscal year 1975. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for these coalbeds only. The delivered coal was sampled at destination in accordance with instructions furnished by the Bureau of Mines, and all samples were analyzed in the Bureau laboratory at Pittsburgh.

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