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By T. L. Marchewka

As part of its program to conserve the Nation's natural resources by developing improved performance materials, the Bureau of Mines, U.S. Department of the Interior, in cooperation with the U.S. Department of Energy, has conducted an investigation of materials of construction able to withstand the high temperature and hostile environments encountered in coal gasification units. Refractory pipe liners are required when extremely hot gases or abrasive solids are transported between processing units in the gasification plants. One promising technique for producing refractory pipe (or refractory pipe liners) is centrifugal casting. For this study, the effect of processing variables such as workability, additives, reinforcement and spinning time, and centrifugal force were evaluated using four commercial refractory concretes. In addition, data on characteristics such as strength, density, abrasion, and spalling resistance of 5-inch-diam refractory pipe were developed. Techniques for forming large-diameter (19-inch) refractory pipe also were evaluated. The test results indicated that all four refractory concretes could be made into strong, homogeneous pipe, but that optimum casting parameters had to be determined for each specific composition. The investigation revealed that the major controlling factor in the production of the centrifugally cast pipe was the workability of the refractory concrete.

Jan 1, 1979

By David M. Hopstock

To help assure an adequate supply of minerals to meet the Nation's economic and strategic needs, the Bureau of Mines is conducting bench-and pilot-scale research using wet high-intensity magnetic (WHIM) separation to recover iron from oxidized taconites of the. Lake Superior region. The advantages and disadvantages of WHIM separation in relation to other separation methods, the most recent innovations in WHIM flowsheet design, and the role of mathematical models in process optimization are discussed.

Jan 1, 1979

By J. M. Singer

Thermal, mechanical, and physical properties of virgin and heat-treated Pittsburgh seam coal were determined as part of a comprehensive study of combustion of monolithic coal block. The information was sought to help characterize pyrolysis and combustion processes in underground coal mine fires but should also prove useful in the study of in situ and surface coal gasifiers. Measured properties include thermal conductivity, specific heat, thermal expansion, density, compressive and tensile strength, porosity, and permeability. The transport property data were obtained (when feasible) in two mutually perpendicular directions of the anisotropic virgin coal material, and coal samples carbonized for 5 hours at temperatures of 350° C, 475° C, 500° C, 650° C, and 850° C. Other coals (Pocahontas No. 3, Sewell, and Illinois No. 6 seams) were investigated for porosity and relative permeability. Interdependence among all properties was evident from the results; however, only a few correlations could be developed owing to inhomogeneity of coal material and specimen variation, which had the effect of reducing the accuracy of measurement and increasing data scatter.

Jan 1, 1979

By John L. Ellenberger

The Bureau of Mines investigated the occurrence of slickensides in mine roof in the Pittsburgh coalbed in a portion of the Valley Camp No.3 mine in southwestern Pennsylvania to improve the potential for prediction of slicken-sided zones and determine the orientations of the most prominent slickensided planes. Two distinct types of slickensides were identified; those which were associated with clay veins observed in the coalbed (genetic), and those which were unrelated to any visible structure (nongenetic). The study draws three conclusions: (1) Nongenetic slickensides are not the result of tectonic forces, (2) both genetic and nongenetic slickensides tend to dip at an angle of 30°, and (3) genetic slickensides tend to be alined parallel to the trend of the clay vein and usually dip toward the center of the clay vein. A schematic roof bolting plan is presented that may provide improved roof support where slickensides are present. Roof stability could be improved by supplemental bolting in the direction normal to the plane of slickensides.

Jan 1, 1979

By J. M. Gomes

The Bureau of Mines, as part of an effort to maximize minerals and metals recovery from domestic resources, has investigated the feasibility of recovering heavy minerals as byproducts from sand and gravel, placer gold, and industrial mineral operations in northern California. Sand samples from about 50 locations were treated by gravity separation to yield heavy-mineral concentrates (black sands). Mineral compositions of the concentrates were determined by chemical analysis and mineralogical examination. Individual zircon, ilmenite, magnetite, platinum-group metals, thoria, and silica products were prepared from heavy-mineral concentrates by selective separation using low-and high-intensity magnetic, high-tension, and flotation equipment.

Jan 1, 1979

By William J. Campbell

This Bureau of Mines report describes a study conducted to determine the relationship of mineral habit to particle size and shape characteristics for prismatic, acicular, fibrous, and asbestiform varieties of tremolite. Particle measurements were made with the petrographic microscope at X 1,250 and the scanning electron microscope at magnifications up to X 10,000. All of the varieties of tremolite, upon Wiley milling, produced a significant percentage of particles that meet the Federal regulatory criteria for counting as asbestos fibers. However, only the asbestiform variety gave milled particles that fell into a size range of >10 µm in length and <0.5 µm in width; some medical scientists consider this range significant for production of adverse health effects.

Jan 1, 1979

By S. J. Hussey

A jig tailing with gold content ranging from 0.33 to 0.43 oz/ton was leached in weak cyanide solution with extractions of up to 97 pct in 24 hours. By countercurrent batch leaching studies and laboratory pilot plant operation, minus 10- plus 20-mesh and minus 6- plus 16-mesh coconut carbon were loaded to 700 oz/ton of Au. Minor silver in the ore reported in the carbon in amounts of up to 100 oz/ton. Gold adsorption rate data and an equilibrium adsorption curve for minus 10- plus 20-mesh carbon at ambient temperatures were developed and used in the successful application of a cascade design theory. The work was performed as a part of the overall Bureau of Mines research effort to help maintain an adequate domestic supply of metals by making improvements in mineral-processing technology.

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 G. R. Palmer

The Bureau of mines evaluated the elution of uranyl carbonate from a strong base resin with a mixed carbonate eluant in a fluidized system. The system consisted of a multiple-compartment ion-exchange (MCIX) elution column with a continuous flow of solution, except for short periods when the resin increments were withdrawn. The exchange of uranyl carbonate from the mill-loaded strong base resin with an eluant composed of 1.0 [M] NaaCOs plus 1.0 [M] NH4HCO3 was studied. The effects of solution flow rate, aqueous-to-resin flow ratio, column diameter, compartment height, initial resin concentration, and column length were examined. The experimental data indicate that for the eluant examined, a resin residence time of 240 minutes is necessary to attain 90-percent elution efficiency. Also provided is a technique for sizing an elution MCIX column form pilot plant experimental data.

Jan 1, 1979

By Richard G. Sandberg

The Bureau of Mins, U.S. Department of the Interior, is investigating a hydrometallurgical procedure to conserve cobalt, nickel, and copper by recovering the metals from the matte byproducts of smelting Missouri lead ores. For want of adequate processing technology the mattes are now either unmarketable or marginally so. The procedure involves leaching with manganese dioxide and sulfuric acid to obtain copper, nickel, cobalt, lead, and manganese sulfates, and elemental sulfur as expressed by the following reaction: MS + MnO2 + 2H2SO4 ? MSO4 + MnS04 + S° + 2H2O, where M = Cu, Ni, Co, and Pb. The leach solutions, containing near theoretical amounts of sulfuric acid and manganese dioxide at 85° to 100° C, convert up to 98 pct of the cobalt, nickel, and copper in the mattes to sulfates in less than 2 hr. As they are formed, the cobalt, nickel, and copper sulfates are dissolved leaving a residue of lead sulfate, lead, sulfur, and gangue. The soluble metals are recovered from the leach solutions by caustic and sulfide precipitation, and the residue returned to the smelter for lead recovery. The manganese can be reclaimed from the spent leach liquor as manganese oxide and recycled to leaching.

Jan 1, 1979

By N. A. Gokcen

In this Bureau of Mines report, appropriate equations correlating the activity of water with the activities of electrolytes in binary and multicomponent solutions have been derived for computer calculation. It was found that the half-integer power series are far superior to the integer power series, for both types of series having the same number of terms. The pro-posed method of calculation is capable of accurately yielding the activities of all components from the measurements of the activity of a single component at various concentrations. This method replaces the cumbersome and objection-able method of graphical integration of the Gibbs-Duhem equation. Two novel methods are proposed for determination of activities of electrolyte solutions important in hydrometallurgy; (1) Water vapor pressure measurement by differential pressure transducers having an accuracy of 0.001 pet, and (2) transpiration method with an inert gas bubbled through concentrated solutions followed by the analysis of the evaporated and redissolved electrolytes with specific ion electrodes having a sensitivity of ±10-10 molal. The first method is suitable for nonvolatile electrolytes, and the second, for volatile electrolytes such as hydrogen halides, HN03, H2S03, etc. The existing methods of estimation of ionic activities have been surveyed, and the best method has been selected, discussed, and summarized.

Jan 1, 1979

By Yael Miron

Ammonium nitrate-fuel oil (AN-FO) mixtures are used as blasting agents in mining pyrite-bearing ores. The temperature of these ores can increase by the continuous, though at times slow, oxidation weathering of the pyrites. At elevated temperatures, AN-FO reacts exothermally with pyrite, and the reaction becomes self-sustained at 120° C ± 10° C. The Bureau of Mines has conducted an investigation to determine the reactivity of mixtures of AN-FO with pyrite containing ferrous sulfate. The results of tests in a heated vessel simulating a hot borehole demonstrate that small amounts of ferrous sulfate, a major product of pyrite weathering, initiate a self-sustained exothermic reaction with AN-FO at 80° C. Five pct by weight of urea was found sufficient to prevent a reaction among the three ingredients, at least within the limits of the test, which reached 180° C. Smaller amounts of urea and of potassium oxalate slowed down the reaction and delayed its onset to higher temperatures, but did not prevent it.

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 George N. Aul

This report describes a method developed by the Bureau of Mines for sealing horizontal degasification holes so that they do not create a gas explosion hazard when intercepted by mining. A cement slurry is pumped into the hole through an injection pipe that extends to the back of the hole. Pumping continues until the slurry returns through the annulus to the hole collar. The hole is then shut in and the grout allowed to harden. Application of the procedure to six horizontal degasification holes at Eastern Associated Coal Corp.&apos;s Honey Run shaft is discussed.

Jan 1, 1979

By L. H. Wullstein

Bureau of Mines research on methods for reclaiming land disturbed by the minerals sector of the economy has produced a specific procedure for effectively germinating seed of Indian ricegrass, a drought-tolerant plant valuable for reclaiming arid and semiarid sites. This report describes the procedure which consists of acid-treating the seed followed by temperature and light cycling treatments. Use of the procedure resulted in an average germination rate of 29 percent, ranging from 18 to 56 percent. Seed subjected to long cold treatment but with acid treatment yielded an average germination rate of 9.2 percent, ranging from 6.6 to 14.7 percent. Untreated seeds (controls) gave germination rates less than 0.1 percent.

Jan 1, 1979

By D. M. Soboroff

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 conducting research on a method for the economic inplant recycling of these waste etchants. Trivalent chromium, produced when the etchant reacts with a sub¬strate, 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 T. J. Driscoll

In this Bureau of Mines investigation, the electrochemical polarization behavior of Fe and Fe-1BCr has been characterized in rigorously controlled 1[N] H2S04 solutions stirred with oxygen or an inert gas. Samples that under-went various levels of corrosion or passivation were examined using Auger electron spectroscopy (AES) and ion sputtering. Passivation of iron occurred at a potential of approximately 0.6 volt (1) in poorly stirred, oxygen-saturated solutions for forward polarization (scanning from cathodic to anodic potentials); (2) in pH-adjusted (increased), well-stirred, oxygen-saturated solutions for forward polarization; and (3) in well~ and poorly stirred, oxygen-and helium-saturated solutions for reverse polarization. Passivation of Fe-18Cr occurred at a potential of approximately -0.1 volt in helium-, nitrogen-, and oxygen-saturated solutions for all cases of forward polarization and most cases of reverse polarization. Elemental depth profiles obtained from AES sputtering measurements indicated that films or adsorbed species were present on iron samples in solution subjected to open-circuit, active, and transpassive corrosion, cathodic reduction, and passivation. This conclusion was reached by considering the distribution of the solution species, primarily sulfur, in the films, which were composed primarily of iron and oxygen. Sulfur was present throughout the films on actively corroding samples, in the outer regions of films of passive and transpassive samples, and on the film surfaces of open-circuit and cathodically reduced samples. For Fe-18Cr, sulfur was found on the surfaces of films on passive samples only, indicating that only the passive samples had films on their surfaces in solution. The films on electropolished and passive Fe-1BCr samples had the largest chromium concentrations, estimated to be approximately 45 at. pct, with less chromium in films of cathodically reduced, active, and open-circuit samples, in that order.

Jan 1, 1979

By R. R. Brown

The solubility and the activity of aluminum chloride hexahydrate, A1C13?6H2O, in aqueous solutions were determined as a part of the Bureau of Mines, U.S. Department of the Interior, research to improve mineral processing technology for recovering alumina from low-grade domestic resources. The solubility of A1C13 in pure water was found to be 31.09 and 31.77 wt-pct at 25° and 85° C, respectively, and decreased drastically to 10 and 0.1 wt-pct when the respective amounts of 20.3 and 37 wt-pct hydrochloric acid (HCI) were added in solution. The equilibrium constant for the solubility of hexahydrate, activities, and activity coefficients of A1C13 and H2O were calculated and compared with the results from the available methods of estimation. The results were shown to be useful in leaching nonbauxitic ores for extraction of alumina by changing the solubilities of component salts upon addition of HC1. Simultaneous solubilities of A1C13, FeC13, KC1, and NaC1 in solutions of HC1-H2O were also determined and their effects on the purity of A1C13?6H20 crystallized from mixed salt solutions are briefly discussed.

Jan 1, 1979

By David C. Oyler, Paul W. Jeran, William P. Diamond

The Bureau of Mines is cooperating with the U.S. Department of Energy in a directional degasification project at the Emerald mine near Waynesburg, Pa. This project is designed to combine the highly successful underground horizontal degasification technology with surface drilling methods. The objective of this program is to demonstrate that directional drilling can be used as a technique for degasifying coalbeds ahead of mining to reduce the hazards of methane-air explosions in coal mines. The directional hole at the Emerald mine is designed to start vertically and enter the Pittsburgh coalbed horizontally. A 3-inch-pilot hole entered the Pittsburgh coalbecl at a vertical depth of 999 feet, The hole will be reamed to 8-3/4 inches in diameter, and 5-1/2-inch casing will be cemented in place. Three individual 3-inch-diameter, 3,000-foot horizontal gas collection holes will be drilled into the coalbed in a “bird foot” pattern. A corehole and vertical dewatering hole have been completed at the anticipated coalbed intercept. The dewatering hole was drilled to130 feet below the Pittsburgh coalbed, a depth of 900 feet, and 880 feet of 7-inch-OD casing was cemented in place. Seven vertical holes for monitoring the extent and progress of degasification have been drilled within the horizontal drilling area.

Jan 1, 1979

By David C. Oyler

The Bureau of Mines is cooperating with the U.S. Department of Energy in a directional degasification project at the Emerald mine near Waynesburg, Pa. This project is designed to combine the highly successful underground horizontal degasification technology with surface drilling methods. The objective of this program is to demonstrate that directional drilling can be used as a technique for degasifying coalbeds ahead of mining to reduce the hazards of methane-air explosions in coal mines. The directional hole at the Emerald mine is designed to start vertically and enter the Pittsburgh coalbed horizontally. A 3-inch-pilot hole entered the Pittsburgh coalbed at a vertical depth of 999 feet. The hole will be reamed to 8-3/4 inches in diameter, and 5-1/2-inch casing will be cemented in place. Three individual 3-inch-diameter, 3,000-foot horizontal gas collection holes will be drilled into the coalbed in a "bird foot" pattern. A corehole and vertical dewatering hole have been completed at the anticipated coalbed intercept. The dewatering hole was drilled to 130 feet below the Pittsburgh coalbed, a depth of 900 feet, and 880 feet of 7-inch-OD casing was cemented in place. Seven vertical holes for monitoring the extent and progress of degasification have been drilled within the horizontal drilling area.

Jan 1, 1979