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By S. Ralph Austin

This Bureau of Mines investigation determined the effects of so-called annealing at high temperatures on radon-222 emanation from domestic uranium ores. Concurrently, a method was developed for closely estimating the emanation coefficients of hot samples from measurements of their gamma activity after cooling. Emanation coefficients of 102 samples from 14 domestic areas of past, present, and possible future uranium production were investigated using modifications of the closed-can, gamma-only assay method at and after cooling from 100° to 1,000° C. True annealing probably does not occur below 500° C. In limited investigations at 500° C and above, effects of annealing are masked by the effects of other parameters. Emanation is commonly less at one or more of the steps investigated in the 100° to 500° C range than before heating. This decrease is tentatively attributed to water loss at temperatures dependent upon the minerals present. The average sample emanates least at 300° C; emanation increases with higher temperatures to at least 900° C. Emanation decreases sharply on cooling, but it is partially restored by prolonged exposure to the atmosphere at room temperature. Higher than average emanation of coffinite ores at 500° C and above may be related to destruction of the coffinite crystal structure.

Jan 1, 1979

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 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 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 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 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 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 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 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 Philip Thompson

A part of the Bureau of Mines mission is to help improve the Nation&apos;s mineral posture by providing the technology for utilizing low-grade ores. In this regard, laboratory testing by the Bureau of Mines has shown that the removal of insoluble slimes using selective flocculation and flotation is a viable method for treating low-grade potash ores that have a high content of water-insoluble impurities. Results indicated that over 82 percent of the insoluble slimes could be removed from sylvinite ore containing 5 percent water insolubles and 13 percent K20 by using nonionic or cationic polyacrylamide flocculants and cationic, anionic, and/or nonionic collectors. Subsequent potash flotation recovered 87 percent of the potash in rougher concentrates containing 57 percent K2O. Sizing and cleaner flotation of the rougher concentrates upgraded the products to 60 percent K2O. Filtration of the water-leached insoluble-slimes flotation concentrates on a bed consisting of leached insoluble-slimes concentrate mixed with potash flotation tailings recovered 80 percent of the brine. Filtration rates using the mixed bed were nine times faster than filtration rates obtained when the insoluble-slimes flotation concentrates were filtered separately.

Jan 1, 1979

By R. H. Nafziger

Bureau of Mines research has shown that very low-sulfur pressure vessel steels with improved mechanical properties can be prepared by two melting processes. Four pressure vessel steels having sulfur contents ranging from 0.0008 to 0.0040 wt-pct, were produced by the electric-arc furnace or by the electroslag processes. Calcium carbide was used as a desulfurizer in the electricarc furnace. Fluxes containing at least 40 wt-pct CaO provided sufficient desulfurization during electroslag remelting. Element recoveries were higher for electroslag remelting than for metal melted in the electric-arc furnace. Bar rolled from electroslag-remelted ingots generally possessed higher tensile strengths and ductility than bar rolled from it t melted in the electric-arc furnace. Charpy V-Notch upper shelf energies were also improved as a result of electroslag remelting. The primary failure mode during impact testing was was microvoid coalescence. Sulfide inclusions were minimal, especially in the electroslag-remelted material.

Jan 1, 1979

By A. B. Campbell

The Bureau of Mines is developing alloys using ion implantation as an alternative to bulk alloys that consume large quantities of strategic materials such as chromium and nickel. These alloys are formed at the outer layer of relatively common materials. To more fully understand the corrosion characteristics and physical properties of this outer layer, it was necessary to deter-mine the alloy concentration as a function of depth into the substrate material. Also, since many of the ion-implanted alloys would be utilized at elevated temperatures, it was necessary to determine the diffusion behavior of the implanted element. Proton-induced X-ray emission and inert gas ion sputtering have been utilized to generate composition depth profiles for Fe-Cr, Fe-Ni, and Fe-AI ion implanted alloys fabricated by implanting 25-kev Cr+, Ni+, or AI+ into iron substrates. The data were fitted (utilizing a computer program) with symmetrical Gaussian profiles yielding values for the range and range straggle of the ions. These parameters were then compared with those calculated from theory. Changes in the profiles due to annealing were investigated and values for the diffusion coefficient were obtained assuming diffusion according to Fick&apos;s Law. For the Cr+ and Ni+ implantation, the profiles as-implanted agree reason-ably well with theory and exhibit ?norrmal" diffusion characteristics at 500° C. For the Al+ implantation, the profile as-implanted is much broader than predicted and exhibits substantial enhanced diffusion at temperatures up to 500° C.

Jan 1, 1979

By H. J. Heinen

To maximize productivity through improved minerals processing technology, the U.S. Department of the Interior, Bureau of Mines, is investigating particle agglomeration techniques as a means of increasing the percolation rates of leach solutions in heap leaching of clayey gold-silver ores. Simulated heap leach experiments were conducted on 50-pound charges of ore that were contained in 5.5-inch-diameter columns, 5 feet in height. Results indicated that the percolation rate of cyanide leach solution could be enhanced markedly by mixing the ore with controlled amounts of lime, flocculants, and water, and then aging the mixture prior to the column leach step. Experimental results obtained on 20-mesh silver tailings and gold ore crushed to 3/8 inch and to 1 inch showed that it was possible to increase percolation rates as much as 100-fold without sacrificing silver-gold extraction. Larger scale tests conducted in 24-inch-diameter, 16-foot-high columns closely paralleled bench-scale results. By improving percolation leaching, these techniques have the potential of helping to solve environmental problems associated with tailings disposal as well as making an important economic impact on gold-silver recovery operations. Investigations are continuing to develop binders superior to lime for particle agglomeration pretreatment.

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