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By M. Hertzberg

The Bureau of Mines measured the energy requirements for the spark ig-nition in air of Pittsburgh seam bituminous coal dust, lycopodium spores, and polyethylene powder with a 1.2-L furnace and 8-L and 20-L chambers. Thermal autoignition temperatures of the same dusts were mea-sured in the 1.2-L furnace. Electrical ignition requirements are given in terms of both effective spark gap energies, [ ] and stored circuit energies, 1/2 CE2. The measured order of electrical ignitability for the three dusts is consistent with the data of other researchers; however, the absolute values are systematically higher, probably because of higher flow and turbulence levels in the chambers used and lower electrical efficiency in the circuit used here. The temperature dependence of the lean limit of flammability for lyco-podium was measured wi th the 1.2-L sys tem, and those measurements con--firm the applicability of the modified Burgess-Wheeler law to a dust. Due to experimental complexities, the minimum ignition energies for dusts may not reflect intrinsic flammability behavior. However, some valuable information may be obtained from the relative ignition energies of various dusts at ambient and elevated temperatures. In addition, the concept of minimum electrical ignition energies for homogeneous gas mixtures is reevaluated theoretically.

Jan 1, 1985

The Bureau of Mines evaluated short-delay coal mine detonators manu-factured by three domestic companies for electrostatic sensitivity, strength, and no-fire current level. Electrostatic sensitivity was studied in pin-to-pin and pin-to-case modes employing lO-kV potential. Strength of detonation was measured in the Bureau's underwater test fa-cility. No-fire current was measured using a constant-current power supply unit. Test procedures and experimental data are included.

Jan 1, 1985

By Wallace W. Roepke

Research to evaluate the lubricity effects achieved by spraying water on the cutting bit of a mining machine or spraying water on the coal during cutting has shown that neither practice affects cutting forces, as had been believed. However, when water was supplied to the cutting zone axially through the bit at 3,000 to 5,000 psi pressure, tangent'ial cutting forces were reduced an average of 30 pct at a I-in depth of cut while normal bit forces were reduced an average of 65 pct. Lower normal forces mean reduced bit wear, faster advance with greater depth of cut, and fewer coal fines.

Jan 1, 1985

By J. M. Stuve

In this Bureau of Mines investigation, the low-temperature heat capacities of polycrystalline phases corresponding to the sulfide compounds CoSO?89' CoS1?33, and CoS2 were measured by adiabatic calorimetry within the nominal temperature range 5 to 300 K. The derived absolute entropies S298 were 10.36±O.02, 12.96±O.03, and 16.31±O.03 cal?mol-1?K-l, respectively, assuming third-law behavior. In addition, the standard enthalpy of formation 8Hf298 of CoSO?89 was determined by bromine solution calorimetry. The derived value of 8Hf298 was -50.63±2.1 kcal?mol-1, based on the 8Hf298 of Co0. This result is considerably more negative than previously published formation values based on high-temperature gas equilibrium studies.

Jan 1, 1985

By Larry A. Haas

The Bureau of Mines is investigating the use of complex gas mixtures, such as would be produced by coal gasification, for reducing iron oxide pellets. A semiempirical model was developed to predict a priori the reduction rate of an iron oxide pellet in a laboratory tube furnace with simulated coal gases at a total pressure of 1 atm. The model uses partial pressures of H2, CO, CO2, CH4 (methane), water vapor, and a temperature-dependent term to predict the rate of reaction. The reduction rate (weight loss per unit of time) was determined with a thermo-gravimetric apparatus (TGA) in the temperature range of 800° to 1,100° C. The ranking of the reductants, in order of decreasing reducing potential, is H2, CO, and CH4 at temperatures between 800° and 1,000° C; however, CH4 became a better reductant than CO at 1,100° C. Water vapor did not decrease the reduction rate as much as did CO2, Carbon deposition was observed at temperatures below 1,000° C with gas mixtures with high CO and low H2 concentrations. With low-Btu gas at 900° C, over 90 pct of the iron oxide was reduced to iron in less than 3 h. This com-pares with a reduction time of 1.5 h with medium-Btu gas and 1 h with reformed natural gases.

Jan 1, 1985

By Kim B. Shedd

The Bureau of Mines measured fiber dimensions on crocidolites (riebeckite-asbestos and magnesioriebeckite-asbestos) from the world's four crocidolite mining regions. The objective of the study was to determine whether there are measurable morphological differences between crocidolite fibers that correlate with the high reported incidence of mesothelioma in miners and mill employees in the Cape Province of South Africa and Western Australia, as compared with little or no reported incidence of this cancer in the Transvaal Province of South Africa or Bolivia. Fiber dimensions measured with the scanning transmission elec-tron microscope showed that crocidolites from Western Australia and the Cape Province have more thin fibers than crocidolites from Bolivia and the Transvaal Province.

Jan 1, 1985

By G. A. Smyres

The Bureau of Mines investigated a HCI-02 leaching procedure to recover Cu, Ni, and Co from a low-grade bulk sulfide flotation concentrate prepared from the Duluth gabbro complex. Since the Duluth gabbro complex is the largest known and unexploited Ni resource in the United States, the development of options for extracting the metal values from the flotation concentrate of this domestic resource is necessary. Conditions were determined for producing a pregnant solution low in Fe to facilitate recovery of the metal values. Leaching experiments were conducted at 15 pct solids, 1000 to 1200 C, 0.2 to 0.3 g HCI per gram concentrate in a 50-gal reactor pressurized to 50 pSig with 02. Base metal extractions from the concentrate were, in percent, 90 to 92 Cu, 99 Ni, 97 to 99 Co, and 0.1 .Fe. Precious metals extractions were erratic and unpredictable; at best their extractions were, in percent, 55 Au, 90 Ag, 40 Pt, and 45 Pd. The reaction time at 1200 C was 0.5 h. The use of compressed air instead of 02 as the oxidant was also investigated. Solvent extraction using LIX 622 was used to remove Cu from the pregnant solution. Cementation on Cu was tested for precious metals recovery, while sulfide precipitation was used to produce a Ni-Co product. A conceptual flowsheet for treating the Duluth gabbro concentrate is proposed.

Jan 1, 1985

By K. E. Soroka

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 coal 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 1,0000 C (1,832° F), and could be recovered for the production of steam, hot water, process heat, or electricity. The Bureau's first held 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's and was surface mined in the 1940'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 fifth 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 1, 3, 4, and 5.) Part 3 describes the instrumentation used to control and monitor the progress of the burnout operation. Parts 4 and 5 deal with the closeout phase of the field demonstration. Part 4 describes the procedure used to quench the fire, and this part (part 5) describes 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-fume exhaustion is a potentially effective method for cooling large underground fire zones. Further investigations of both Burnout Control and the water-injection-fume exhaustion quenching procedure are planned.

Jan 1, 1986

By G. W. Elger

The Bureau of Mines investigated the conversion, at both laboratory and pilot plant scale, of a low-grade ilmenite to chlorination-grade feedstock that could substitute for imported rutile used to produce titanium tetrachloride. The concentrate was derived from the Tahawus, NY, lode deposit of ilmenite-magnetite in rock that contains anorthosite and gabbro. Charges of the ilmenite concentrate, containing 46.6 wt pct Ti02 blended with soda ash, were carbothermically reduced in an electric arc furnace, which separated most of the iron and left a high-titanium slag. However, the slag contained Ca, Mg, and Mn constituents that rendered the material unsuitable for continuous chlorination by causing plugging problems. After being ground and pelletized, the slag was reacted with S02 and air at 7000 to 9000 C, which selectively converted the harmful impurities to soluble compounds that were removed in a subsequent water or dilute HCI leach. In laboratory tests, the combined levels of harmful impurities were decreased from 5 to as low as 0.5 wt pct in leached slags. In pilot plant tests, leached slags sulfated at a rate of 10 lb/h averaged 85.5 wt pct Ti02 with pertinent impurity levels averaging 1.86 wt pct. The leached slag was successfully chlorinated in a laboratory fluidized-bed reactor at 9500 C to extract titanium as TiCI4.

Jan 1, 1986

By R. J. Morrell

The Bureau of Mines conducted a series of laboratory experiments to test a cutting technique for hard rock using large-scale drag cutters. Cutting experiments were performed on rocks ranging in compressive strength from 10,000 to 27,000 Ib/in2, using large drag cutters from 3 to 6 in. in width. The tests were conducted on a special test apparatus, called a ripper tester, which made a curvilinear cut across the rock sample while measuring the cutting force acting on the drag cutter. The cutting method that evolved from these experiments is called ripper cutting, and its energy efficiency appears superior to all other large-scale mechanical fragmentation techniques. In addition, the method cre-ated very little dust, and the wear on the bits was negligible. A fragmentation system based on ripper cutting was then devised, and a large-scale test device was fabricated to allow full-scale laboratory testing of the system. The results of these tests will be published in future Bureau reports.

Jan 1, 1986

By Ronald H. Church

The Bureau of Mines tested & ground penetrating radar (GPR) system in the central Florida phosphate district. to determine the feasibility of utilizing GPR technology for subsurface cavity detection. The test area is located in karst topography where sinkhole development is prevalent. State regulations require subsurface drilling of damsites to identify underground anomalies; however, this method is not totally accurate in locating subsurface cavities that could lead to sinkhole development. An electromagnetic method of identifying anoma-lous subsurface conditions could reduce or eliminate the possibility of dam failure due to sinkhole development. The Bureau devised a GPR system that successfully penetrated over 50 ft of overburden and gave recognizable radar return signals characteristic of a rock-cavity interface.

Jan 1, 1986

By David P. Lindroth

The objective of this research by the Bureau of Mines was to determine the technical feasibility and associated pilot data for drying minus 1/4-in coal with microwave energy at a frequency of 2.45 GHz. The drying data were obtained experimentally on three coal types: bituminous, subbituminous, and lignite. The experiments were performed with a custom-designed conveyorized microwave oven having a continuous power capability of 12 kW. Drying efficiencies near the theoretical maximum of 1.54 kg of water per kilowatt hour of energy input were achieved for two coals and two sizes; overall drying efficiencies averaged 77 pct.

Jan 1, 1986

By Noel N. Moebs

This report summarizes a Bureau of Mines study on the use of geotechnology to identify and reduce ground control hazards at slate quarry operations in eastern Pennsylvania. The major ground control hazard is falling rock, attributed to weathered bedding plane faults, which weaken quarry highwalls. It was demonstrated that these faults can be detected outside of the quarry perimeter using surface resistivity measurements. Falls of ice from quarry highwalls constitute a second major hazard, which requires water diversion as a basic control method. In situ stresses seemingly cause only minor problems in slate extraction although they could interact with developed stresses and lead to failure of barriers between quarries. Pull tests showed that rockbolts anchor firmly in slate and should prove effective in securing loose rock.

Jan 1, 1986

By Charles Seitz

The Bureau of Mines has modified its parts-per-billion helium-4 analyzer to improve the analytical capabilities of the instrument. The modifications resulted in the following improvements: (1) The analytical precision of the instrument for 10 consecutive analyses was improved to ±1 ppb at the 5,000-ppb helium-4 level, (2) the helium-4 sensitivity was increased almost tenfold, and (3) the minimum detectable limit for helium-4 was improved to 0.5 ppb. The modifications made to improve the instrument included replacing the ion-source control circuit with a direct-current solid-state design, controlling the temperature of the ion source, stabilizing and reducing the pumping rate of the vacuum system, and optimizing peak integration.

Jan 1, 1986

By James 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, were evaluated: two red shale, two fireclay, one silicon carbide, one silica, one carbon, and one high-alumina. Samples were exposed to 10 wt pct H2S04 at 50° C and 10, 30, 50, 70, and 90 wt pct H2S04 at 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were observed in the silicon carbide and car-bon materials. Weight changes and the leach rate of Al, Ca. Fe. K, Mg, Na. Si, and Ti were also monitored. The most severe corrosion conditions were at 90° C and 30 to 50 wt pct H2S04 for the acidproof and at 10 wt pct H2S04 for the acid-resistant materials. The silica and the high-alumina materials were the most acid-resistant, followed by the higher density red shale and fireclay.

Jan 1, 1986

By Rustu S. Kalyoncu

Nonoxide ceramics with improved high-temperature properties could substitute for high-temperature alloys and reduce toe Nation's dependence on imports of Cr, Co, Ni, and Mn. To meet this objective, the Bureau of Mines conducted research to synthesize u1trafine reactive boron nitride (BN) powders BN powders were prepared at temperatures ranging from -75? to 750? C. Low-temperature reactions (-75? to 200? C) between boron halides and N compounds led to formation of e1emento-organic compounds that were thermally decomposed to u1trafine (approximately 100-to 150-A particle size) reactive BN powders. BN powders were also prepared through the reaction of a 10w-me1tinginorganic B compound (boric acid, borax) with an organic N compound (carbimide and thiocarbimide) in N2 and/or ammonia (NH3) atmospheres at temperatures between 500? and 750? C.

Jan 1, 1986

By N. Greninger

The Bureau of Mines examined the possibility of a seasonal variation of respirable dust concentration in U.S. coal mines. The first step was to review company and MSHA-inspector dust samples that had been collected during the past several years in 14 selected mines for compliance purposes. Results indicated severe scatter in data; most standard deviations of the dust concentrations measured in winter and summer months were comparable in magnitude with the mean values of dust concentrations for the seasons. Therefore, a detailed statistical analysis was conducted. At the 90% confidence level, the company samples of three mines had winter means 0.15 to 0.54 mg/m3 higher than the summer means; six mines had negligible seasonal variations; and five mines had winter means that ranged from higher to lower than the summer means. Inspector data, however, were too sparse for analysis. In view of both the low frequency of occurrence of a seasonal effect and its wide scatter in several of the mines, the study was ended with the conclusion that seasonal varia-tion in respirable dust levels, in general, is an insignificant factor.

Jan 1, 1986

By M. J. Ferrante

Relative enthalpies of high-purity disodium hexatitanate (Na2Ti6013) were measured at the Bureau of Mines to provide new thermodynamic data needed to advance the technology of materials. Measurements from 298.15 to 1,478 K were made by drop calorimetry with a copper block. Tabulated values are listed for the standard relative enthalpy, heat capacity, en-tropy, and Gibbs energy function between 298.15 and 1,500 K. Enthalpy data are also given in equation form and are combined with thermodynamic data from the literature to derive values of standard enthalpies of formation, Gibbs energies of formation, and logarithms of the equilibrium constants of formation. Similar calculations were made for the reaction of Na20 with Ti02.

Jan 1, 1986

By G. A. Smyres

A GaC12--B2 l-eachtng procedure and meEal-recovery method for treating an arsenical Cu-Co sulfide concentrate was developed by the Bureau of Mines as an alternative to smelting, which is no longer considered an environmentally acceptable method for treating arsenic-containing ores. The procedure involved leaching in a CaC12 solution with CaC03 for 96 h at 26 pct solids (concentrate and CaC03), 1150 C, and a pressure of 50 psig (345 kPa) with oxygen. More than 98 pct of the cobalt and 97 pct of the copper were extracted, and 99.98 pct of the arsenic and 99.9 pct of the iron remained in the leached residue. A filtration rate of 2.9 gal/(ft2.h) [118 L/(m2.h)] and a cake formation rate of 36 Ib/(ft2.h) [172 kg/(m2.h)] were obtained by filtering reacted pulp at 1000 C. More than 99 pct of the copper in the pregnant solution was extracted as CuCl2 by golvent extraction with a new copper extractant. Copper was stripped from the loaded organic with a sulfate-chloride solution, which was used as the anolyte for electrowinning of copper in a membrane cell. Copper plate produced was more than 99.99 pct pure and requi.red 0.81 (kW'h)/lb Cu [1.78 (kW·h)/kg Cu]. Cobalt sulfide was precipitated at pH 3 with Ca(HS)2.

Jan 1, 1986

By R. G. Sandberg

The Bureau of Mines investigated a hydrometallurgical procedure to recover gold, silver, and byproduct lead from a complex lead-zinc sulfide ore. A ferric chloride (FeCI3) preleach, at 40° C in 6 h, extracted about 50 pct of the zinc and formed insoluble silver and lead chlorides. Subsequent acid thiourea leaching, for 1 to 3 h at 40° C, extracted about 85 pct of the gold and silver. Lead chloride was solubilized from the remaining residue with NaCI brine solution at 55° C in 1 h. Lead metal was recovered from the brine solution in an electrolytic cell with an anion perms elective membrane at a current efficiency of 95 pct and current density of 100 A/m2. Spent FeCl3 leach solution was reoxidized in the anode compartment at a current efficiency between 75 and 95 pct.

Jan 1, 1986