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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

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.'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'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'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

By Robert C. Gabler

Evaluation of incinerated sewage sludge as a secondary resource for aluminum, phosphorus, and minor constituents such as copper and zinc was initiated as part of the Bureau of Mines secondary resource program. The elemental composition of sludge ash for 14 plants in 11 U.S. cities was determined. Comparing industrialized cities with cities where most of the sewage is domestic, significant differences in heavy metal content were noted. Various parameters were investigated affecting the extraction of metals and phosphorus from a typical industrial city sludge ash and from a Palo Alto, Calif., sludge ash with a high precious metal content. Three extraction-recovery procedures for metals and phosphorus using sulfuric acid leaching, ion exchange, and various precipitation techniques were investigated. The last procedure developed was a combination approach using a three-stage countercurrent sulfuric acid leach that recovered most of the economic values from the sludge ash and also removed the leachable fraction of elements of environmental concern.

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 Robert P. Vinson, Fred N. Kissell, Edward D. Thimons

Because of the high number of accidental methane gas ignitions in metal and nonmetal mines, the Bureau of Mines searched for a simple guideline that would allow mine personnel to evaluate the methane hazard in a given mine. Air samples were collected by the Bureau in 53 metal and nonmetal mines and analyzed for trace evidence of methane gas. Samples were collected in the returns and at the working faces. Those mines classified as gassy by the Mine Safety and Health Administration had a significantly higher average methane concentration than those classified as nongassy. Of the 9 gassy mines sampled, 7 had methane concentrations above 100 ppm, whereas only 1 of the 44 nongassy mines had a concentration above 100 ppm. The 100-ppm concentration may be used as a simple and convenient guideline for forecasting the methane hazard in a mine, whether or not the mine is classified as gassy. There was no consistent correlation between commodity mined and methane concentration, nor was there a correlation between mine depth and methane concentration. Neither of these factors can be considered a guideline for predicting methane hazards.

Jan 1, 1979

By Edward D. Thimons

Because of the high number of accidental methane gas ignitions in metal and nonmetal mines, the Bureau of Mines searched for a simple guideline that would allow mine personnel to evaluate the methane hazard in a given mine. Air samples were collected by the Bureau in 53 metal and nonmetal mines and analyzed for trace evidence of methane gas. Samples were collected in the returns and at the working faces. Those mines classified as gassy by the Mine Safety and Health Administration had a significantly higher average methane concentration than those classified as nongassy. Of the 9 gassy mines sampled, 7 had methane concentrations above 100 ppm, whereas only 1 of the 44 nongassy mines had a concentration above 100 ppm. The 100-ppm concentration may be used as a simple and convenient guideline for forecasting the methane hazard in a mine, whether or not the mine is classified as gassy. There was no consistent correlation between commodity mined and methane concentration, nor was there a correlation between mine depth and methane concentration. Neither of these factors can be considered a guideline for predicting methane hazards.

Jan 1, 1979

By I. L. Nichols

Laboratory characterization studies have investigated the processing variability of carbonaceous uranium-bearing materials found in-sandstone deposits. This work was conducted by the Federal Bureau of Mines in support of its goal to maintain an adequate supply of minerals to meet national economic and strategic needs. Conventional processing produces only partial uranium recovery from these ore materials. Ore samples from New Mexico, Texas, and Wyoming were examined, and each responded differently. Using direct acid leaching techniques, some of the ores required acid additions of only 50 pounds per ton, while others required 300 pounds per ton of material. Maximum extractions ranged from 83 to 94 percent in the six ores tested. Roasting those ores prior to leaching improved extraction of the uranium to the 90 to 99 percent range. An oxidative autoclave treatment used with five of these ores resulted in extraction of 78 to 97 percent of the uranium. The experimental studies also showed that some carbonaceous materials can be concentrated by froth flotation. The flotation tailings were amenable to acid leaching, and up to 98 percent of the uranium was extracted from this type of material.

Jan 1, 1979