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By B. T. Brady

Recent theoretical, experimental, and field studies conducted by the Bureau of Mines suggest that rock failures may be predicted and, in some instances, controlled. Theoretical studies that were later corroborated by laboratory and field studies predict that a seismic anomaly will precede rock bursts and/or roof falls in mines. The seismic anomaly is predicted to consist of an increase in the number of seismic events occurring in the immediate vicinity where the failure 1s nucleated. This increase will then be followed by a dramatic decrease of seismicity in a broad region that surrounds the location of the impending failure. The dimensions of this region allow a preliminary estimate of the time to failure (measured from the time the seismicity increase began) as well as an estimate of the energy that will be released at the instant of failure. Field observations indicating that this predicted behavior does precede rock bursts and a roof fall are presented in this report. Implications of results to the problem of failure control in mines that experience massive rock failures are discussed.

Jan 1, 1978

By Peter F. Steidl

Seven degasification wells have been completed in the Pittsburgh coalbed at the new Emerald mine near Waynesburg, Pa. Funding was provided by the Bureau of Mines to perform stimulation treatments on five of the wells, to show that this is a feasible and economical means of degasifying part of a coalbed. The seven wells ranged in depth from 590 to 910 feet. Stimulation treatments used 25,260 to 42,660 gallons of foam and 7,400 to 12,800 pounds of 20/40-mesh prop sand. Pumping rates were 10.8 to 11.6 bbl/min and treating pressures were from 1,050 to 1,600 psig. On the day following stimulation, gas production ranged from a few hundred cubic feet per day to more than 100,000 cu ft/day.

Jan 1, 1978

By E. F. Divers

This Bureau of Mines report describes the results of a program to develop small, rugged mechanical dust collectors (scrubbers) with high dust collection efficiency and low energy comsumption for controlling dust in coal mining operations. All of the scrubbers described are similar in configuration and are powered by 6-hp, 2,000-ft3/min vane axial fans. Air pressure differential is less than 6 inches water column. Height of the scrubbers? including fan is less than 14 inches, width is less than 16 inches, and length is less than 45 inches. The flooded fibrous-bed scrubber achieved respirable (less than approximatey 7 µm) dust collection efficiencies of 95 percent. The small-diameter-cyclone scrubbers showed about 92 percent efficiency and can be best where excess water is a problem. The wetted brush scrubber showed 88 percent efficiency at low cost, and the wetted fan scrubber showed a slightly lower efficiency (87 percent) but offered the smallest size and cost. A suitable water droplet eliminator is described.

Jan 1, 1978

By I. Liebman

The Bureau of Mines conducted research to develop triggered barrier systems for protection against gas explosions that can occur in underground coal mines during the use of continuous miners. Several extinguishing agents were tested in barriers at a simulated mine face. Water, powered by pressurized nitrogen, was found to be efficient in stopping fully developed gas explosions, but it had little effect against the explosion during its incipient stage. Hybrid combinations of currently known extinguishants, however, were successful against incipient explosions. Three hybrids that were developed and tested consisted of Halon 1301, combined with either an aqueous foam solution, water, or a dry chemical powder. The three hybrids were found to be more efficient than any constituent alone. Results of the tests point to a synergism between the hybrid components, and indicate that the Halon aids in dispersing its constituent and also converts the aqueous foam solution into a stable fine foam and the water into fine drops.

Jan 1, 1978

By V. R. Miller

The Bureau of Mines developed and evaluated a detecting and sorting device to separate the copper-bearing portion from the barren portion of Michigan native copper ore in the minus 4- plus 1-inch size range. Small-scale sorting tests were also conducted on minus 1- plus 1/2-inch material from the Centennial No. 6 mine, using a previously developed system that was modified to increase sensitivity. Results showed that, with the added sensitivity, 85 to 90 pct of the copper in the minus 1- plus 1/2-inch material could be recovered in about 50 to 60 pct of the fraction. Sorting tests on minus 4- plus 2-inch and minus 2- plus 1-inch fractions from the Centennial mine were conducted with the large sorting system. Results showed that 86 to 93 pct of the copper was recovered in 43 to 64 wt-pct of the sorted fractions. Combining of concentrates from the two fractions resulted in a recovery of 90 pct of the Popper in 55 pct of the weight. The composite concentrate contained 2.40 pct copper, and the tailing analyzed 0.33 pct Cu; the head sample assayed 1.46 pct Cu.

Jan 1, 1978

By Frank G. Horino

Drill cores from 18 exploratory holes that were drilled into the unleached saline beds were tested for mechanical properties by the Bureau of Mines. Test cores were primarily selected from zones L4B, R4B, L3, and R3A in the Piceance Creek Basin, Rio Blanco County, Colo. Regression analysis techniques were tried in an attempt to relate kerogen yield or apparent specific gravity to the parameters compressive strength, Young's modulus, and Poisson's ratio. Correlation coefficients were very poor, indicating that this type of analysis was not amenable to these data. Analysis of variance techniques were tried using a division of either greater than or less than 10% nahcolite together with the requirement of less than 3% dawsonite. Results showed that a larger percentage of nahcolite tended to lower the compressive strength and to increase Young's modulus. A second analysis was made using a division of less than 3% dawsonite and greater than 3% dawsonite together with the requirement of less than 1% nahcolite. For this analysis, a larger per-centage of dawsonite tended to increase compressive strength, Young's modulus, and Poisson's ratio. Mean compressive strength values were determined for the mining horizons of interest. Average physical properties for design purposes were also determined for the horizons of interest and for a proposed adit based only on logged geologic depths to these horizons. No consideration was given to percentages of nahcolite and dawsonite. Creep data obtained from nahcolite-and dawsonite-rich oil shales provides a best fit to a modified power equation.

Jan 1, 1978

By Calvin K. Lee

This Bureau of Mines report describes a simple fire-retardant treatment for wood. The treatment involves preheating the wood surface at high heat flux (~0.6 cal/cm2 sec) to form an in situ surface char layer (~3 mm thick) on the wood. Laboratory-scale fire tests show that the precharring technique improves the fire-resistance of virgin wood by decreasing and delaying generation of volatile gases through thermal insulation effect of the surface prechar layer.

Jan 1, 1978

By Seth C. Schaefer

As part of the Bureau of Mines, U.S. Department of the Interior, effort to provide thermodynamic data for the advancement of minerals technology, the Gibbs energy of formation of sphalerite (zinc sulfide) was investigated with a high-temperature galvanic cell employing stabilized zirconia as the electrolyte. In the temperature range 948 to 1,210 K, potential measurements were obtained for the cell Pt, ZnS + ZnO, S02 = 1 atm // Zr02 // Cu20 + Cu, Pt, with the overall cell reaction ZnS(c) + 3 Cu20(c) = ZnO(c) + 6 Cu(c) + S02(g). (1) These results, combined with the best available values of ?Gf° for ZnO, S02, and Cu20 from the literature, give the Gibbs energy of formation of zinc sulfide for the reaction Zn(l,v) + 1/2 S2(g) = ZnS© (2) ?Gf° = -64.223 + 24.02 X 10-3T ± 0.650 kcal/mole (3) (948-1,180 K; standard states - pure liquid zinc and S2 gas at 1 atm), and ?Gf° = -92.720 + 48.17 X 10-3 ± 0.650 kcal/mole (1,180-1,210 K; standard states - pure zinc vapor and S2 gas at 1 atm). A third law analysis yields for the formation reaction Zn(1) + 1/2 S2(g) = ZnS(c), (5) a standard enthalpy of formation as follows: ?Hf298.15 = -63.64 ± 0.700 kcal/mole.

Jan 1, 1978

By Richard G. Sandberg

Sphalerite concentrates prepared during processing of Missouri lead ores contain small percentages of cobalt and nickel which adversely affect zinc electrolysis. The Bureau of Mines has evaluated solvent extraction and precipitation techniques to remove and recover cobalt and nickel from zinc sulfate solution prior to zinc electrolysis. Prepared zinc sulfate solutions containing about 190 gpl of zinc and 50 ppm of both cobalt and nickel were treated using various combinations of complexing reagents, solvent, pH, concentration, time, and temperature. The following complexing reagents gave the best results: a-nitroso-ß-naphthol, ß-nitroso-a-naphthol, 1,2 cyclohexane dione dioxime (nioxime), di-2-pyridyl ketone oxime, and dimethylglyoxime. These reagents in suitable solvents lowered the cobalt and nickel levels to <0.1 ppm. Stripping the complexed reagents from the solvents was not possible except for nioxime. Direct addition of the appropriate reagent to the prepared zinc sulfate solution resulted in the precipitation of cobalt and nickel. Several possible flowsheets are presented for the removal and recovery of cobalt and nickel. Good zinc deposits were successfully electrowon from zinc sulfate solutions purified by solvent extraction and precipitation.

Jan 1, 1978

By David R. Flinn

This Bureau of Mines report describes methods to electrodeposit erosion-resistant titanium diboride coatings from molten alkali metal borate baths at 900° C. These coatings have been shown to be highly resistant to material loss during impingement with high-velocity alumina and silicon carbide powders, and they show promise as protective coatings to reduce metal loss in erosive chemical environments, such as coal gasification systems. The most erosion-resistant coatings were prepared on nickel, Inconel, and molybdenum from an electrolyte containing LiBO2, NaBO2, Na2Ti03, and TiO2. The best coatings were deposited at current densities of [~]20 ma/cm2, using titanium or titanium diboride anodes. Erosion-resistant coatings were shown to exhibit (1) a high degree of crystallographic orientation along the (100) or (110) planes, (2) a chromium impurity level of less than 3 pct, and (3) a uniform, smooth, consolidated surface appearance when viewed under a microscope or by scanning electron microscopy. Optical spectroscopic studies of the molten electrolyte suggest that the lower valent (+3) titanium ion predominates in the baths.

Jan 1, 1979

By A. T. Iannacchione

The Bureau of Mines established geologic factors affecting the mining of the Lower Kittanning coalbed to aid in coalbed minability studies and examined the occurrence of "wants" (places where coal is missing) and types of unstable roof rock strata. Trends established from mapping, including prediction of areas of high methane emissions, were extrapolated to unmined areas. &apos;Wants&apos; in the coalbed are of two types: Erosional and depositional. Erosional features occur where north-south-trending sand-filled channels cut into the coalbed. Variations in depositional environments have caused the coalbed to "split" into several thinner units. Slickensides, commonly indicative of unstable roof, are adjacent to and on the underside of sandstone channels; they were caused by differential compaction and by soft sediment sliding along the contact between the sandstone and adjacent shale. The frequency of unstable roof also increases where the interval between the Middle and Lower Kittanning coalbed is less than 30 feet. The zones of weakness at the contacts above and below the Middle Kittanning coalbed are the controlling factors for unstable roof in these strata. Methane emissions from the coalbed are controlled primarily by depth, fracture permeability, and rank of coal. Local geologic factors are coalbed thickness, associated rock strata, structure, and proximity to outcrop.

Jan 1, 1979

By C. D. Messelt

The Bureau of Mines investigated the application of a diffusion model to sintering rate data developed for lithium titanium ferrite. The data were obtained by sintering pressed pellets under identical conditions for various times up to 11 hours. Stereological measurements were made on polished sections, and sintering rates were calculated. A model for intermediate stage sintering was fitted to the stereological data. This procedure produced a method by which these type data could be used to study the relative importance of volume and grain-boundary diffusion under a variety of sintering conditions.

Jan 1, 1979

By Laird Crocker

A goal of the Federal Bureau of Mines is to minimize the undersirable environmental conflicts and impacts associated with mineral processing operations. To help reach this goal the Bureau operated a citrate-process pilot plant for the removal of sulfur dioxide from lead smelter sintering machine waste gases to test the process. The process uses a carboxylate solution such as citric acid to absorb sulfur dioxide from waste gases. The absorbed sulfur dioxide is subsequently reacted with hydrogen sulfide to precipitate sulfur and regenerate the solution for recycle. Nominal capacity of the pilot plant was 1,000 scfm of 0.5 vol-pct sulfur dioxide gas. The pilot plant was operated for over 5,400 hr and produced about 55 net tons of sulfur. The operation demonstrated that (1) 99 pct of the sulfur dioxide could be removed from lead smelter sintering machining waste gases containing from 0.1 to 0.6 vol-pct sulfur dioxide, (2) sulfur precipitation and solution regeneration with hydrogen sulfide in conventional stirred vessels was readily controlled, (3) precipitated sulfur could be continuously recovered as a 99.S-pct-pure product by flotation and melting, and (4) 78 dry-vol-pct hydrogen sulfide gas could be produced from pilot-plant product sulfur, natural gas, and steam.

Jan 1, 1979

By William J. Karwoski

To improve rock-burst control in deep vein mining, a field demonstration has been carried out by the Bureau of Mines to test a new rock-burst control concept--rock preconditioning in advance of mining. The procedure is to fracture the major rock-burst-prone zone during the development of each level before production mining. This allows initial mining to begin in a preconditioned zone and later mining from the level below to end in a prefractured or preconditioned pillar zone that is relatively burst-free. This full-scale field demonstration was carried out On the 7700 level of the Hecla Mining Co.&apos;s Star-Morning mine. An expected burst-prone zone along the main vein between 7 and 10 crosscuts, some 250 feet long by 40 feet above and below the level, was preconditioned by blasting a fanlike ring of drilled holes from each crosscut. The drill holes, up to 100 feet long and 4 inches in diameter, were loaded with high explosives and shot. About 4,550 feet of drilling and 9,000 pounds of explosives were involved in the effort. Comparison of preshot and postshot data from monitoring instrumentation indicated that the blasting did fracture the rock in the planned zone and did result in an immediate stress decrease and softening of rock. The field data compared favorably with predicted results from a finite-element computer model simulation of the destressing. Based on observations made during mining and on the data from the Hecla rock-burst monitoring system, there is no doubt that this preconditioning in advance of mining demonstration resulted in much-improved rock-burst control during first-floor mining. It was also concluded that preconditioning the vein was more effective than preconditioning the wall rock.

Jan 1, 1979

By M. M. Tilman

Etchants containing hexavalent chromium and sulfuric acid are used in a variety of surface-finishing operations. When the resultant spent solutions are discarded, substantial quantities of chromium are lost and pollution prob¬lems are created. To minimize the undesirable environmental effects while improving metal and minerals recycling technology, the Bureau of Mines is con¬ducting research on a method for the economic inplant recycling of these waste etchants. Trivalent chromium, produced when the etchant reacts with a substrate, is oxidized in the anode chamber of a diaphragm cell; other metals, dissolved during the etching operation, are transferred to the catholyte. When waste brass etchants are treated in this manner, all of the trivalent chromium is oxidized and more than 40 percent of the copper and zinc is removed. Similar copper removal and chromium oxidation are achieved with waste printed circuit board etchants and rinse waters from plastic etching operations. The electrical energy needed to regenerate 1 kg sodium dichromate is less than 9 kwhr. Regenerated brass etchants evaluated by two companies equaled or exceeded the performance of fresh etchants.

Jan 1, 1979

By J. L. Holman

The Bureau of Mines has extended its previous development of cast Mn-Cu damping alloys to powder metallurgy (P/M) consolidation of alloys containing 55 to 75 wt-pct Mn. Blends of minus 200-mesh elemental powders were compacted cold in directional and isostatic presses. With 1 pct binder, typical green densities ranged between 76 and 80 pct of theoretical when pressing at 30 or 48 tsi. Green strength increased with compacting pressure and copper content. As-sintered tensile strengths ranged to 60,000 psi fox a hydrogen, sintered 60Mn-40Cu alloy, along with 5-pct elongation. Sintered densities ranged between 90 and 96 pct of theoretical. Sintering (a as effective when holding for 1 hr at maximum temperatures of 900° to 1,040` C, dependent on composition. Strength and ductility were considerably lower than for equiva¬lent cast alloys. When aged to the damping condition, alloys containing 60 to 70 pct Mn exhibited >40 pct specific damping capacity (SDC) at 5,000-psi stress, considerably higher than values reported for equivalent cast material. Effects of 1 or 3 pct Sn or Zn additions on SDC and other properties were assessed. Trials were conducted on consolidating rings and gears of the 65Mn-35Cu alloy on industrial-type P/M equipment.

Jan 1, 1979

By J. T. McLendon

As part of its research project in developing improved refractory materials for metallurgical applications, the Federal Bureau of Mines obtained hot modulus of rupture data at 1,500°,1,550°, and 1,600° C on samples of 13 refractory periclase materials produced from seawater, lake brines, and natural magnesite. The periclase samples also were characterized to establish chemical and mineralogical composition and microstructure. The results indicated that a high MgO content does not necessarily assure good hot strength and that an optimum and varying CaO-Si02 ratio exists for each individual periclase sample.

Jan 1, 1979

By I. Liebman

Two triggered barrier systems and several extinguishing agents were tested against coal dust explosion propagating in the main entry of the Bureau of Mines Experimental Mine at Bruceton, Pa. One system used a high-pressure cylinder to propel the extinguishant; the second system used pressurized nitro-gas or Halon 1301 (CF3Br) in a low-pressure system to power the disperser. The relative efficiencies of the extinguishants were determined by compar¬ing calculated concentrations of the extinguishant clouds present in the mine during suppressing of the explosions. Results showed the following trend of increasing effectiveness: Purple-K (KHC03)<water<hybrids consisting of foam or water combined with Halon 1301<Halon alone. On a weight basis, water was two to three times as efficient as Purple-K, whereas the hybrids and Halon alone were only marginally superior to water. Maximum efficiency of an extinguishant is attained by high rates of discharge from the barrier and by minimizing the time interval between onset of discharge and flame arrival to that necessary for discharge. Both the high- and low-pressure barrier systems were demonstrated to be capable of suppressing coal dust explosions; however, because of the potential hazard of the former, the low-pressure system is considered to be the most attractive prototype.

Jan 1, 1979

By Harold L. Rhodes

The Bureau of Mines has developed a method for determining the H2S content in natural gas samples. A gas chromatograph with a flame photometric detector was used to analyze samples with H2S concentrations ranging from 5,000 ppm to a minimum detectable limit of 0.01 ppm. A mass spectrometer was used to analyze samples containing H2S in amounts greater than 5,000 ppm. Methods are presented for preparing containers for H2S samples and for preparing standards using partial pressure and weighed standard methods, Sample collection techniques are discussed, as are analytical results which illustrate the loss of H2S while in the sample container and provide a basis for evaluating containers used for sampling and standard preparation.

Jan 1, 1979

By C. B. Davison

One goal of the Bureau of Mines is to conserve the Nation&apos;s mineral resources by developing improved performance materials. Consistent with this goal, the Bureau conducted studies on the formation of undesirable cristobalite in seven different fire clays used as refractories. The studies employed scanning electron micrography, chemical and X-ray analyses, and pyrometric cone equivalent determinations to examine the sample clays and determine the effect of thermal history and stablilizing additives on the amount of cristobalite in various calcines. This research has indicated that as fire clay calcining temperatures increased from 1390° to 1,490° C there was a gradual decrease in the percent of cristobalite present in the calcines and a progressive development of mullite crystallization. No cristobalite was found in fire clays calcined above 1,550° C, but cristobalite reappeared when the calcines were reheated to temperatures between 1,400° and 1,500° C. The research also revealed that additions of lithium fluoride (LiF) prevented formation of cristobalite in fire clay calcines.

Jan 1, 1979