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By G. B. Atkinson

The Bureau of Mines investigated a method for increasing the leaching rate of bulk superalloy scrap to facilitate recycling and recovery of critical metals such as Ni, Co, and Cr. Three superalloys were investi- gated, the cast-nickel-base superalloy IN-738, the wrought-nickel-base superalloy Rene-41, and the cast-cobalt-base superalloy Mar-M-509. Superalloys melted with 20, 30, 40, and 50 pct Al metal to form inter- metallic compounds were easily crushed to a convenient particle size and reacted rapidly with acid solutions which dissolved the metals. For example, leaching 1/2-in pieces of unalloyed IN-738 with excess 6N HC1 at 95° C for 2 h dissolved about 0.5 pct, while leaching 10 g of minus 20-mesh 30 pct Al-70 pct IN-738 with excess 6N HC1 at 95° C for 2 h dis- solved 96.2 pct.

Jan 1, 1983

By Richard S. Olsen

Prior work by the Bureau of Mines demonstrated a feed preparation method that eliminates the formation of slime during leaching of calcined kaolinitic clay and makes leached residues fast settling and easy to filter. Nitric acid leaching rates determined for calcined kaolinitic clay prepared by this method were found to correspond to a zero-order reaction model for both batch and continuous, stirred-tank leach-ing. A rate constant of 0.136 min-1 was determined. Separation of solid residues from the reacted slurry was examined, and filtration rates were determined. Permeabilities of the flocculated, leached residues were around 51 darcys, or 5.0 x 10-7 cm2 for laminar flow through 4-ft-deep beds.

Jan 1, 1983

By J. E. Schiller

The Bureau of Mines is investigating methods to treat waste water that contains cyanide. This report describes a new method that removes heavy metals and all forms of cyanide. In the first step, hydrogen peroxide and sodium thiosulfate are added at pH 7 to 9 in a 1:2 molar ratio to convert free and weakly complexed cyanide to nontoxic thiocyanate. Then steryldimethylbenzylammonium chloride is added to precipitate ferro-cyanide, and finally, ferric sulfate is added as a sweep floc and sequestrant for heavy metals. After the suspended solids settle, the water is polished by filtering. The water initially contained 1 to 5 mg/L Fe, 1 to 5 mg/L Cu, and 10 to 30 mg/L total cyanide; the level of each of these constituents was reduced to less than 0.02 mg/L.

Jan 1, 1983

By K. J. Ladwig

The Bureau of Mines conducted a field investigation of the water quality in inundated underground coal mines in the Northern Anthracite Field, eastern Pennsylvania. Water samples were collected at multiple depths from nine abandoned mine shafts in the Wyoming Basin, ranging from 68 to 650 m (223 to 2,132 ft) in depth and intersecting as many as seven mined seams in a single shaft. The shafts were also monitored for fluid resistivity, fluid temperature, Eh, and pH using downhole instrumentation. The monitoring program showed that the formerly highly acidic mine water is now slightly alkaline. Sulfate concentrations decreased as much as 74 pct in the flooded workings and 54 pct at a mine water discharge from values reported in 1964 and 1968, respectively. These data are consistent with the inhibition of pyrite oxidation and gradual flushing of oxidation products in flooded mine environments. The monitoring program also revealed significant vertical stratification in water quality in five of the nine shafts, each characterized by two easily recognizable zones. The transitions between zones were sharp, marked by rapid changes in Eh, pH, and ionic composition, the upper zones being less contaminated than the lower zones. The development of stratification appears to be a function of shallow localized flow conditions, arising primarily from the relative positions of mine openings and structural features of the coalbeds.

Jan 1, 1984

By Eugene Baker, Joseph Cervik, Albert Sainato

In Europe, water infusion is used widely to reduce generation of respirable dust during mining. Its use in the United States is limited to a few plow operations in the Pocahontas No. 3 Coalbed. This Bureau of Mines report describes the technology for infusing water in to a longwall panel and reports the results of a recent demonstration in the Lower Sunnyside Coalbed that achieved dust reductions averaging 58 pct. Because water infusion increases moisture content of the coalbed, face air velocities in excess of 500 ft/min (2.5 m/s) are possible, further diluting dust levels before dust entrainment occurs. An economic analysis shows a 23-pct reduction in operating costs when coal production is increased by changing from unidirectional mining to bidirectional mining with water infusion.

Jan 1, 1983

By Nicholas Kyriazi

The Bureau of Mines subjected three commercial compressed-oxygen self-contained self-rescuers to a series of laboratory treatments designed to simulate various environmental conditions in underground coal mines. The environmental treatments consisted of extremes of temperature and of shock and vibration. The tests were designed to predict the ability of the self-rescuers to withstand those environmental stresses without causing a decrease in wearer protection. A critical concern was internal damage to an apparatus that would cause it to malfunction or seriously degrade its performance without any obvious external signs. The Bureau has previously tested chemical oxygen self-contained self-rescuers in a similar research program. Although the three compressed-oxygen units are not as sturdy as the chemical oxygen self-rescuers tested previously, they performed reliably after treatments on treadmill tests with human subjects and on machine tests using a breathing and metabolic simulator. Serious damage was caused by both the heat treat-ment of 71° C (venting of the 02 bottle in most cases), and in the shock treatment (breaking open of the case and dislodging of the components). When physical damage is obvious, a complete refurbishing of the damaged self-rescuer is recommended.

Jan 1, 1983

By R. E. Siemens, Gary L. Hundley

The Bureau of Mines has devised and demonstrated a process for recovering Ni and Co from low-grade domestic laterites . The process consists of four mmaajjoorr steps : ( 1 ) reduction roast , ( 2 ) ammoniacal leach , ( 3 ) solvent extraction , and ( 4 ) electrowinning . Several solid - liquid separation steps are required that affect the economics of the overall process . In this study , two techniques for solid - liquid separation , centrifugation and thickening , were investigated . This report presents the results of ( 1 ) laboratory and pilot plant studies to determine parameters for sizing centrifuges and thickeners and ( 2 ) an economic study of the two techniques , based on the requirements of a commercial - size ( 5,000 - tpd ) laterite processing plant . Sizing and other equipment - related recommendations , based on data from the Bureau's studies , were obtained from commercial manufacturers . The costs of thickening and centrifugation , including all the unit operations affected , were determined by the Bureau's process evaluation group . The total operating costs for separation using the two techniques ( including depreciation on the capital cost of equipment ) were found to be quite close : $ 17.26 per ton of laterite for centrifugation and $ 18.15 per ton of laterite for thickening . For centrifugal separation , the greatest cost was found to be the initial capital cost for the separation equipment ; using thickeners , the greatest cost was for reagent recovery .

Jan 1, 1983

By S. J. Schatzel, J. Cervik, A. A. Campoli

The cross-measure borehole technique is being studied by the Bureau of Mines as an alternative to the use of surface gob boreholes as a means of controlling methane in gobs during longwall mining. Small-diameter holes are drilled from underground locations into strata overlying the mined coalbed. When the roof strata are fractured by the mining opera- tion, a partial vacuum applied to the boreholes draws the methane out of the fractured strata and prevents it from entering the mine ventilation system. Tests in the Upper Kittanning Coalbed showed that 50 pct of the methane produced by the longwall mining operation was captured by the cross-measure boreholes. Borehole inclination and penetration into the gob are two important borehole parameters that affect the performance of the cross-measure borehole system.

Jan 1, 1983

By David C. Oyler

Methane-drainage holes must be completely filled by grout before mining to prevent the emission of large quantities of gas during mine-through, which would constitute an explosion hazard. In November 1980, seven horizontal holes at the multipurpose borehole, a small-diameter shaft drilled as a Bureau of Mines coalbed methane-drainage installation on the property of the Federal No. 2 Mine, Monongalia County, WV, were plugged using a sodium silicate gel grout. This report de- scribes the grout mix and the use of the grout at the multipurpose borehole, and discusses the results observed upon mine-through of the holes in early 1981. Cost data for the sodium silicate grout are also presented.

Jan 1, 1984

By R. H. Church, William E. Webb, Walter E. Pittman, James R. Boyle

As part of the Bureau of Mines health and safety research program, a short-range locator system, capable of locating miners who have become trapped following a mine accident, has been devised, The system consists of a lightweight, low-power radio transmitter incorporated into a miner's cap lamp battery and a directional receiver carried by rescuers. Prototype transmitters have been constructed, and the propagation of their signals has been investigated, The detectability of the signal in underground coal mines has also been investigated, This research indicates that a short-range location system would serve as an economical and practical means of locating miners from within the mine following an accident,

Jan 1, 1984

By Arthur V. Petty

The Bureau of Mines has investigated the effect of refractory oxide additions, introduced in soluble form, on the refractory properties of 42-, 58-, and 70-pct-A1203 brick. Brick having porosities ranging from 12 to 16 pct were impregnated with solutions containing chrome, chrome-iron, zirconium, calcium, magnesium, cobalt, nickel, tin, and manganese ions. Additions of some of these ions provided dramatic improvements to such properties as hot modulus of rupture, hot load, and particularly slag resistance. These improvements can be related to reduction of porosity, amorphous grain boundary phases, formation of more refractory bond phases, and reduction of the wettability of Al203-containing refractories by metallurgical slags. Fifty-eight-percent-AI203 brick, impregnated with chrome, showed hot modulus of rupture, hot load, and slag resistance two to five times better than those of untreated 70-pct-AI203 brick. This could result in reducing the Nation's dependence on imported refractory-grade bauxite generally required for high-A1203 brick, as domestic alumina resouces could be used to produce the improved refractories.

Jan 1, 1984

By D. G. Foot

The Bureau of Mines investigated two methods for recovering potash from carnallite ore in continuous 100-lb/h flotation units. In the insoluble-slimes flotation procedure, insoluble slimes were removed by flotation prior to potash flotation. In the direct flotation method, insoluble slimes were depressed and the potash floated directly without prior removal of the insoluble slimes. Seventy-three percent of the potash in the ore was recovered in a leached final KCl product contain-ing 59.1 pet K20 using the insoluble-slimes flotation method. The direct flotation method recovered 74.5 pct of the potash in a final product containing 60.2 pet K20. The rate of return on the investment was calculated at 13 pct for the insoluble-slimes flotation method and 15 pct for the direct flotation method, based on a Bureau economic evaluation.

Jan 1, 1984

By L. P. Kleinmann

To control the formation of acid drainage at its source, the Bureau of Mines has investigated the role of iron-oxidizing bacteria in the oxidation of pyrite. In laboratory tests, it was determined that Thio-bacillus ferrooxidans could be controlled in coal refuse using anionic surfactants, with an associated decrease in acid production of about 75 pet. Based on these results, large-scale tests were conducted at an 8-acre active coal refuse area in northern West Virginia and an 11-acre inactive refuse pile in southern West Virginia. Acid production was decreased 60 to 95 pet for 4 to 5 months after application of 55 gal/ acre of 30-pct sodium lauryl sulfate solution. To date, effluent surfactant concentrations have been extremely low. Either a hydroseeder or a road-watering truck can be used to apply the surfactant. Since the surfactant solution must reach the pyritic material to be effective, sites that have been reclaimed are generally not amenable to these procedures. A simple laboratory test is described that provides an estimate of adsorption potential; this can be used to calculate a safe application rate.

Jan 1, 1983

By D. J. MacDonald

The Bureau of Mines has conducted bench-scale investigations leading to the design of an integrated process for producing reactor-grade zir-conium oxide (Zr02) from zircon sand, which avoids the air pollution, water pollution, fire hazard, and odor problems associated with the hexone-thiocyanate process. The integrated process consists of three steps: production of crude zirconyl sulfate solution, solvent extraction, and production of Zr02 from strip liquor. This report describes the solvent extraction step. Multistage, countercurrent liquid-liquid extraction with a tertiary amine in kerosine was used to separate zirconium from a dilute H2S04 solution containing hafnium and other impurities. Process steps de-scribed include extraction from an aqueous feed solution to form a hafnium-contaminated, zirconium-bearing organic-phase solution, scrubbing to separate zirconium from coextracted hafnium, stripping to transfer hafnium-free zirconium into an aqueous strip liquor, chloride-loading to produce a chloride-bearing organic solution, scrubbing with the chloride-loaded organic solution to remove traces of uranium impur-ity from the zirconium-bearing strip liquor, and regeneration to pre-pare the organic solution for reuse. These steps were performed simul-taneously in steady-state, bench-scale experiments. Zirconium recovery of up to 93 pct was achieved. Results of an economic evaluation are included.

Jan 1, 1984

By D. J. MacDonald

The Bureau of Mines investigated two alternative methods for treating a zirconium-bearing chloride-sulfate strip liquor to obtain reactor-grade Zr02. One method involves neutralization with NH3 and the other hydrothermal precipitation. The strip liquor was derived from zircon sand by a Bureau of Mines method for separating zirconium and hafnium via solvent extraction with a tertiary amine. Neutralization with NH3 to precipitate hydrous zirconium oxide required 0.9 to 1.1 g NH3 per gram of zirconium. The NH3 can be recovered for recycle. Zr02 that met reactor-grade specifications was produced by precipitation with NH3? Hydrothermal precipitation of Zr02 from strip liquor required that the solution be maintained at 2600 C and 680 psi for 10 min and in a non-corrodible pressure vessel. In bench-scale experiments both methods gave-zirconium recoveries greater than 99 pct.

Jan 1, 1984

By J. P. Bennett

The Bureau of Mines is investigating the acid resistance of ceramic materials to identify construction materials for emerging technology in chemical and metallurgical processes. Eight commercial ceramic materials, including two red shale, two fireclay, a silica, a silicon carbide, a carbon, and a high-alumina brick, were evaluated. Samples were exposed to 40 wt pct HN03 at 70° and 90° C and 60 wt pct HN03 at 50°, 70°, and 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were generally small or not detected, except for a strength drop in the high-alumina brick, which decreased in strength when exposed to the chosen acid concentrations at 90° C. Vol-ume and weight changes were also measured. The leach rates of Al, Ca, Fe, K, Mg, Na, Si, and Ti were monitored. Increasing temperature or a decrease in the acid concentration resulted in an increased ion leach rate. Of the conditions tested, the most severe corrosion occurred at 90° C for a 40-wt-pct-HN03 solution. The silica brick had the best overall acid-resistant properties, followed by a red shale and a fire-clay brick. The carbon and silicon carbide bricks are not recommended for service.

Jan 1, 1984

By Lester M. Adams

In 1980, the Bureau of Mines surveyed a group of mine seals in Randolph County, WV, to evaluate their effectiveness for reducing toxic pollutants in mine water discharges. The survey focused on 11 block wet mine seals, but mine seals of several other types were also examined. The seals were installed in 1966 and 1967 in abandoned drift portals by the Federal Water Quality Administration (FWQA), a predecessor of the Environmental Protection Agency (EPA), in cooperation with the Bureau of Mines and other Federal and State agencies, in a project known as Elkins Mine Drainage Pollution Control Demonstration Project. The seals were designed to prevent air from entering the mine portals while allowing mine water to flow out. It was believed that by preventing air from entering inactive or abandoned mines, the formation of toxic pollutants and acid mine drainage (AMD) could be reduced. Evaluation of the seals was based on water flow measurements, water analyses, and visual observations. The Bureau's 1980 data were compared with past data collected by the EPA. Several leaks and failures were observed in the clay seals, as evidenced by apparent blowouts and the absence of vegetation where the mine water surfaced. Analyses of the 1980 data indicated some improvement in the quality of water discharged from many of the wet air seals.

Jan 1, 1984

By J. W. Sterner

The Bureau of Mines conducted studies on four makes of Japanese automobiles, three 1981 and one 1982 model years, received from three manufacturers to determine if their materials composition would present problems to the current technology used to process junk automobiles for metal recovery. One of each make of automobile was hand-dismantled to determine the materials composition. In addition, two nearly identical automobiles of each make were shredded at a commercial operation where all metal products and rejects were collected for analysis to determine metal and nonmetal distribution. The average weight of the four automobiles to be dismantled, less batteries, tools, and fluids, was 1,938.3 lb. The weight was distributed as 1,472.9 lb. ferrous and 115.6 lb nonferrous metals, 275.2 lb combustibles, 72.3 lb noncombustibles, and 2.3 lb electrical components. The dismantled automobiles, less gas tanks, fluids, tools, wheels, tires, and batteries, which were all removed from the automobiles that were shredded, contained an average of 1,389.1 lb ferrous and 101.6 lb nonferrous metals, 305.7 lb nonmetals, and 2.3 lb electrical components. In comparison, materials collected from the shredded automobiles averaged 1,304 lb ferrous metals, 80 lb nonferrous metals, and 341 lb landfill materials. There were no materials used in the manufacture of the late model Japanese automobiles that should present handling or processing problems to the steelmaking or secondary metal recyclers.

Jan 1, 1984

By A. Y. Lee

Prior work at the Bureau of Mines resulted in the successful development of a bench-scale, combination electrorefining-electrowinning method for recycling the lead from scrap batteries using waste fluosilicic acid (H2SiF6) as electrolyte. This paper describes larger scale experiments. Anodes cast from scrap battery lead were electrorefined in a 20-L multielectrode cell for 3 to 7 days. The anodes, containing 2 to 2.5 pct antimony, were ideal for obtaining firm and adherent slime blankets. Cathode deposits, assaying 99.99 pct Pb, were obtained, with current efficiencies near 99 pct. Sludge leaching was done in 100-L tanks followed by filtering in 61 cm square vacuum pan filtersu Lead of greater than 99.99-pct purity was recovered from the filtrate by electrowinning in a 20-L multielectrode cell using insoluble Pb02-Ti (lead dioxide-coated titanium) anodes and pure lead cathodes. The fluo-silicic acid electrolyte depleted in lead was repeatedly recycled to leach more sludge, and there was no problem with impurity buildup. The amount of Pb02 formed on the anodes during electrowinning was less than 1 pct of the total lead deposited on the cathodes, as long as the phosphorus concentration in the electrolyte was greater than 1.3 giL. Emissions of lead in air were less than 10 ~g/m3, well below the proposed OSHA limit of 50 ~g/m3.

Jan 1, 1984

By R. D. Brown

This Bureau of Mines report describes a new methodology for identifying and sorting scrap metals using two modern portable instruments: a thermoelectric sorter and a hand-held emission spectroscope. The method, tested on a 27-sample stainless steel and superalloy array, makes it possible to group and/or identify a typical mixture of high-value metal scrap in two or three steps, whereas as many as seven or eight steps are needed to perform the same separations using chemical spot tests. A portable fluorescent X-ray analyzer identified 19 of the 27 alloys in the sample array by name or type; these alloys are included in the microprocessor memory. The remaining alloys were identified by using the analyzer in its elemental analysis mode and comparing the results wit.h alloy specification chemistry.

Jan 1, 1984