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By J. P. Bennett

Based on previous Bureau of Mines research indicating that improved high-temperature properties could be achieved for periclase refractories through chemical additions, the Bureau investigated the properties of full-size bricks produced from chemically modified periclase refractory grains and the suitability of making such chemical additions to Mg(OH)2 slurries prior to production of the periclase grains. In full-size brick testing, strength values, both hot and cold, for the optimized bricks were superior to those for a commercial 98-wt-pct-MgO refractory. The best results were obtained for a natural magnesite with an adjusted CaO:Si02 (C:S) ratio of 3.0 and a 1.0-wt-pct addition of Zr02 and for a seawater periclase with an adjusted C:S ratio of 2.5 and a 0.5-wt-pct addition of Mn02. For samples produced from chemically modified Mg(OH)2 slurries, additions of both Mn02 and Zr02 and an increase in C:S ratios produced significant increases in hot flexural strength, similar to those resulting from chemical additions made to periclase grains. The most effective modifications were additions of Mn02 to brine-derived periclases having a C:S ratio adjusted to 3.0. These results on chemically modified magnesia refractories indicate that such material could potentially substitute for magnesiachrome refractories containing imported chromite.

Jan 1, 1984

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 Philip W. Holland

The Bureau of Mines has developed a trace helium analyzer for deter-mining helium-4 in the parts-per-billion range. The instrument is used for analyzing pure gases, laboratory-prepared standards, and atmospher-ic samples. Accuracy at the 95-pct confidence level in the 50-to 20,000-ppb range is within ±2 ppb or ±0.4 pct, whichever is greater. The minimum detectable helium-4 concentration is calculated to be 5 ppb. The analyzer consists of a modified helium leak-detector mass spec-trometer, a laboratory-built sample inlet system, and a liquid-nitrogen-cooled charcoal trap. A programmable integrator and event-control module make automatic operation possible. The portability of the analyzer allows it to be used in the field.

Jan 1, 1984

By Dale E. Wittmer

Nonoxide ceramic materials could substitute for high-temperature alloy steels containing imported critical and strategic materials such as cobalt, chromium, and nickel if their high-temperature properties can be improved. An important result of this substitution would be a reduction of the Nation&apos;s need for imports of critical and strategic materials. In this Bureau of Mines investigation, the primary objective was to produce high-purity u1trafine (particles <5 ~m equivalent spherical diameter (ESD)) alpha-silicon carbide (a-SiC) powders with improved high-temperature properties using the Bureau&apos;s patented turbo-milling process. A secondary objective was to determine the feasibility of using polymer mill construction materials as a means of eliminating metal contamination from the turbomill. U1trafine a-SiC powders with BET (Brunauer-Emmett-Te11er) surface areas from 30 to 35 m2/g (~0.06 ~m particle ESD) were produced in an all-polymer turbomi11. These high-purity powders (with I-pct Band I-pct C additions) hot-pressed to greater than 99 pct of their optimal density and exhibited properties commensurate with those of commercially available a-SiC. The most promising of the construction materials tested for the major wear surfaces of the turbomi11 was u1trahigh-mo1ecu1ar-weight (UHMW) polyethylene, a polymer thermoplastic.

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 J. S. Dunning

Recent developments in energy conversion, mining and minerals processing, pollution control, and chemical equipment have placed in-creased demands on heat-resistant alloys. Higher corrosion rates from oxidation, hot corrosion, and sulfidation have increased consumption of materials that contain critical and strategic minerals and in many cases have limited productivity. The Bureau of Mines is conducting re-search on substitute materials having greater resistance to high-temperature corrosive atmospheres above 6000 C compared to austenitic stainless steels such as AISI 304, 316, and 310, with the goal of conserving critical metals such as Cr and Ni. The substitute materials are based on Fe-Cr-Ni-Al compositions. Aluminum additions to Fe-Cr-Ni alloys significantly improve high-temperature corrosion resistance, particularly sulfidation resistance. In the alloy, devised by Bureau researchers, aluminum additions are held in the form of a second-phase precipitate, 8NiAl. Minor additions of Ti, Mn, and Si improve workability.

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

By G. K. Derby

The Bureau of Mines investigated methods for removing dragline bucket wire rope terminations with the objective of finding efficient methods that are safer than the method most commonly used at U.S. surface mines, which is to use the explosive impact of a projectile fired from a cannon to remove the rope termination. Removal of a wire rope termination for repair or replacement requires separation of the wedge and socket that lock together to secure the rope end. The Bureau investigated currently used methods and improved upon and tested two safer alternate methods for removing wire rope terminations. A cannon test program was conducted, using 40-and 50-gr primer (detonating) cord, to establish the possible force produced with a 4-in-bore cannon and a 55-lb projectile. Wedge and socket units supplied from cooperating mines were separated under controlled conditions to establish data on separation force requirements. The two alternate methods investigated were use of the force generated by (1) a pendulum ram and by (2) a portable hydraulic pusher. Both methods are capable of providing sufficient force to effect wedge and socket separations on draglines with up to 78-yd3 buckets under normal conditions.

Jan 1, 1984

By M. L. Glenn

The Bureau of Mines is conducting research on substitutes for chromium-containing alloys in order to conserve imported critical and strategic materials. Part of this research concentrates on finding low-chromium substitutes for heat-resisting stainless steels for the temperature range 600° to 800° C. Ferritic alloys are emphasized that have oxidation resistance provided by chromium contents as low as 10 pct and stress rupture strength provided by the precipitation of the chi(X)-phase intermetallic compound, (Fe36Cr12 (Mo, Ti)10). Initially, research was concentrated on selecting an alloy composition having a minimum chromium content with strengthening provided by the X-phase. An Fe-(10-12 pct)Cr-6 pct Mo-(1.5-2.0 pct)Ti alloy was selected. After the alloy selection, the tensile, stress rupture, and oxidation properties were determined. Stress rupture properties were found to be similar to those of 304 stainless steel. However, the alloys possessed brittleness during both stress rupture and tensile testing, possibly as a result of too high a content of molybdenum and titanium. Higher than expected oxidation rates were found that may be caused by the high molybdenum content.

Jan 1, 1984

By R. H. Grau, A. Sainato, S. J. Schatzel, T. M. Kohler, A. T. Iannacchione

This Bureau of Mines research study found gas emission rates from an advancing face, and flows and pressure of gas from an exploration drill hole were dependent upon the geology of salt encountered in a domal salt mine. Normal production-grade "pure" salt adjacent to an anomalous&apos; zone was found to have a methane emission rate of less than 5 ft3/ ton (0.1 m3/t) of mined salt from a room advanced by a continuous miner. Extremely low gas flows [less the 4 ft3/h (0.1 m3/h)] and lack of pressure buildup were also observed from this normal salt in a 154-ft (47-m) exploration drill hole. These data indicate that methane emissions should not be a problem when mining in this type of salt. In the adjacent anomalous zone, methane emission rates ranged from 15 to 70 ft3/ton (0.4 to 1.8 m3/t) of mined salt from an advancing face. Gas flows of approximately 42 ft3/h (1.2 m3/h), and pressures in excess of 900 psig (6,200 kPa) were observed in an exploration drill hole when the anomalous zone was encountered. This information suggests a greater methane emission hazard from the anomalous zone than from the associated normal salt. If this trend of increasing emissions problems associated with anomalous zones of salt is common with similar anomalous zones encountered or observed in other domal salt mines, then special control strategies should be employed to minimize this potential mining hazard.

Jan 1, 1984

By Robert F. Chaiken

More than 500 fires are now burning in abandoned coal waste banks and coal deposits in the United States. Once established, such fires can burn for decades, and extinguishing them by conventional methods such as surface sealing to exclude air, excavation to remove fuel, or flushing to cool the fire zone is usually difficult and always expensive. Burnout Control, a technique developed by the Bureau of Mines for the control of abandoned fires, involves the accelerated combustion of coal in place with total management of the heat and fumes produced. A burning waste bank or mine is placed under negative pressure relative to the atmosphere, and heat and combustion products are drawn from the combustion zone through an exhaust ventilation system. Heat produced appears as sensible heat in the exhaust, at temperatures as high as 1,000° C (1,832° F), and can be recovered for the production of steam, hot water, process heat, or electricity. The Bureau&apos;s first field demonstration of Burnout Control was at Calamity Hollow in Allegheny County, PA (near Pittsburgh). Calamity Hollow was the site of an underground mine in the 1900&apos;s and was surface mined in the 1940&apos;s. In the winter of 1961-62, a fire of undetermined origin was discovered in the exposed coal. In 1963, the Bureau constructed a trench barrier around the fire and a surface seal over the affected area. The fire was isolated, but not completely extinguished. In 1979, when the Bureau began work on the Calamity Hollow Mine Fire Project, to demonstrate controlled burnout, the fire was still smoldering on the hot side of the trench barrier. The project, which was begun in December 1979 and ended in July 1982, consisted of the design, construction, operation, and subsequent dismantling of a Burnout Control ventilation system. This report is the fourth in a five-part series that describes the Calamity Hollow Mine Fire Project. The first report, part 1, describes the design and construction of the field installation. Part 2 will present the results of a continuous 4-month burnout operation. (Because part 2 involves the analysis of a substantial body of data, it will not be published until after publication of parts 3, 4, and 5). Part 3 describes the instrumentation used to control and monitor the progress of the burnout operation. This part (part 4) and part 5 both deal with the closeout phase of the field demonstration. The quenching of the fire is described in this report, and part 5 will describe the final excavation and backfilling of the heated zones. The reports in this series document the Calamity Hollow controlled burnout demonstration, which showed that (1) controlled in situ combustion is a feasible method for controlling underground fires in abandoned mines, (2) the resultant thermal exhaust output is sufficient for energy utilization, and (3) water injection with fume exhaustion is a potentially effective method for cooling large underground fire zones. Further trials of both Burnout Control and water injection with fume exhaustion are planned.

Jan 1, 1984

By D. P. Lindroth

The Bureau of Mines is engaged in research on ground probing radars for detection of geologic hazards in advance of mining. Penetration distances and interpretation models depend on the dielectric properties and wave propagation characteristics for coal measure stratified media. Relative dielectric constants and dissipation factors were measured under ambient conditions for Pittsburgh Seam coal measure rock over the frequency range of 20 to 100 MHz by the susceptance-variation method. The rock types measured were representative sedimentary rock located above the Pittsburgh Coal Seam. Extreme values for the computed attenu-ation distance ranged from 1.7 m at 100 MHz for siltstone to 230 m at 20 MHz for a particular limestone.

Jan 1, 1984

By Martin Hertzberg

In this Bureau of Mines study, an equation is derived for the limit burning velocity for divergent, spherical propagation from an ignition kernel of radius, r: (Su)e = ( ) . For flame propagation into a preexisting, stretching velocity gradient of magnitude dv/dx, the limit velocity is (Su)e = (a dv/dx)1/2. These formulations are shown to be equivalent to the fluid dynamic concepts of Damkoh1er, Kar10-vitz, and Markstein. Existing data for the b10woff limits of flames are shown to give excellent agreement with those concepts provided that proper account is taken of two dilution effects: composition dilution caused by entrainment and velocity gradient dilution caused by flow expansion. Approximate flow-field solutions are also derived for the unburned gas motion above an upward propagating, spherical flame kernel in buoyancy-induced flows. It is shown that;, the upward hemisphere propagates toward a stagnation plane in a counterflow configuration involving the balance between the combustion force, which accelerates the cold gas upward, and the buoyancy force that accelerates the cold gas downward. The position of the stagnation plane above the upward propagating hemisphere is related to the ratio of the buoyant velocity, vb, to the burning velocity, Suo Extinction of the upward propagating wave occurs by flame stretch in that counterflow configuration when n = Vb/Su begins to exceed the expansion ratio, Pu/Pb&apos; and the wave is blown off by its own buoyancy-induced flow field.

Jan 1, 1984

By P. R. Bremmer

As part of a program to devise alternative technologies for producing alumina from domestic resources, the Bureau of Mines investigated the leaching of calcined kaolinitic clay to form basic aluminum chloride solutions. Bench-scale experiments were conducted for single-stage batch leaching with AICl3 solution and three-stage countercurrent leaching with substoichiometric HCI. Variable conditions of clay calcination and leaching were studied to determine their effects on aluminum extraction and pregnant liquor composition,

Jan 1, 1984

By R. E. Green

The Bureau of Mines undertook a bench-scale study of three different types of oxidized taconites3 from the Lake Superior district to improve the dispersion-selective flocculation-desliming process for beneficiating these materials. The response-surface contours of the effects of dissolved ionic species in the water and of three dispersion systems on the selective flocculation process were studied. Results of metallurgical data and chemical analyses of the aqueous phase showed that the water quality affects the performance of the selective flocculation process.

Jan 1, 1984

By John Durkin

Electromagnetic narrow-band signals were transmitted through the earth at 27 coal mines located throughout the United States. From those Bureau of Mines tests, apparent earth conductivity values were derived based upon a homogeneous half-space model of the earth. The derived conductivity values were found to be inversely proportional to the transmitted frequency and mine depth. A linear regression model relating the logarithm of the conductivity to the mine depth was formulated, and the results indicate that the mine depth can be an adequate predictor of the apparent earth conductivity above coal mines. Apparent earth conductivity was found to decrease with mine depth.

Jan 1, 1984