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By W. L. Falke

The Bureau of Mines has developed a system that permits the "soft" soldering of aluminum and aluminum alloys with standard tin-lead solders. The method employs application of a thin nickel-copper-alloy coating to the substrate, which enables the tin-lead solders to wet readily and spread over the areas to be joined. With conventional technology, aluminum and aluminum alloys are extremely difficult to solder because tenacious surface oxide films prevent wetting. With the Bureau-developed method, the aluminum substrate is mechanically or chemically cleaned to facilitate bonding to a minute layer of zinc that is subsequently applied with an electroless zincate solution. The nickel-copper-alloy (30 to 70 pct Ni) coating is then applied electrolytically over the zinc, using immersion cell or brush-coating techniques. Development of acetate electrolytes has permitted deposition of the proper alloy coatings. The coated areas can then be readily joined with conventional tin-lead solders and fluxes. The joints so formed are ductile, strong, and relatively corrosion resistant, and exhibit strengths equivalent to those formed on copper and brass when the same solders and fluxes are used. The method has also been employed to soft-solder magnesium alloys.

Jan 1, 1983

By H. C. Ko

Heats of solution of calcium carbon-ate (calcite) and calcium oxide in hydrochloric acid were determined by solution calorimetry. Combination of these two heats yields a value of 42.643±0.024 kcal/mole for the enthalpy of calcination of calcite at 298.15 K. Literature data on ?H°298.15 of calcination of calcite were reviewed and compared. Thermodynamic properties for the calcination process were calculated from 298.15 to 1,500 K using Gibbs energy functions. This research was undertaken by the Bureau of Mines as an effort to provide thermodynamic data for the advancement of minerals technology, energy conservation, and environmental preservation.

Jan 1, 1982

By E. A. Johnson

As part of its effort to reduce the environmental impact associated with mining and metallurgical operations, the Bureau of Mines used a modified form of the Environmental Protection Agency's Extraction Procedure toxicity test on copper reverberatory slags that contained low, medium, and high levels of the impurity elements As, Pb, Sb, Bi, and Zn. All tests resulted in extracts that did not exceed those limits published in the May 19, 1980, Federal Register; there-fore, these solid wastes were designated as nonhazardous for most landfill disposal situations. However, arsenic and lead levels disturbingly close to the allowable limits--and even higher levels of copper and zinc, for which there are no established limits--leached from the high-impurity-element granulated slags. These slags should be handled in such a way so as to minimize the possibility of water contamination. One baghouse dust was tested according to the EPA procedure and found to exceed the extract limits by a factor of 10. This solid waste may be considered hazardous.

Jan 1, 1982

By P. R. Bremner

In keeping with its mission to maximize mineral and metal recovery from domestic sources, the Bureau of Mines investigated a method to extract silver from tailings not amenable to cyanidation. Results of a laboratory study on the recovery of silver from cyanide tailings containing 1.7 ounces of silver per ton by leaching with an acidic ferrous chloride-sodium chloride solution are presented. The effects of reagent concentration and reaction time on the leaching of silver were investigated. A leaching solution containing 5 wt-pct NaCI, 2.5 wt-pct FeCI2, and 1.2 wt-pct HCI (for acidity) extracted 82 pct of the silver from the tailings during a 24-hour leach. The amount of HCI consumed during the leach was 46 pounds of HCI per ton of feed. Only 23 pct of the silver was extracted by conventional cyanidation. Ninety-nine percent of the silver was recovered from the pregnant solution by cementation onto iron powder.

Jan 1, 1982

By James P. Bennett

To improve construction materials for emerging chemical and metallurgical technologies, the Bureau of Mines is investigating the acid resistance of ceramic materials. In the study described here, eight commercial ceramic materials comprising two red shale, two fire clay, a silica, a silicon carbide, a carbon, and a high-alumina brick were evaluated. Samples were exposed to 20 wt-pct HC1 at 50° C for 110 days. The test apparatus designed to evaluate the materials is described. Changes in chemical and mineralogical composition, cold crushing strength, volume, and weight, and leach rates of AI, Ca, Fe, K, Mg, Na, Si, and Ti ions were monitored. In general, the statistically significant physical property changes that occurred were small. In many cases, no changes were detected.

Jan 1, 1982

By David P. Lindroth

The Bureau of Mines has developed and successfully tested a hangup clearance module for use in clearing hangups in underground mine chutes and ore passes. The Bureau's tests showed that the hangup clearance module can be effectively used to clear mine hangups. Furthermore, it is believed that clearance using this module is quicker, safer, and more efficient than the method currently used. The hangup clearance module uses a ballistic disk explosive charge that can clear hangups located as far as 50 feet (15.2 m) from the position where the charge is detonated. Mine personnel can therefore set up the module and the charge it contains without being exposed to dangerous areas. This report describes the principles of operation of the module, provides data and drawings for its construction, and gives instructions for its setup and use. The report also summarizes the development of the module, briefly discusses preliminary and underground tests, and lists the current and potential applications of the hangup clearance module to underground mining.

Jan 1, 1982

By Michael T. Nigbor

The Bureau of Mines assisted the Rocky Mountain Energy Co. in a pilot-scale in situ leaching experiment at Casper, Wyo., to determine if sulfuric acid can be used as a cost-effective alternative lixiviant (leachant) for uranium in situ leaching. This experiment, which lasted more than 2 years, is the first fully documented pilot-scale operation in which the leaching-restoration cycle was completed using sulfuric acid instead of the more common carbonate-bicarbonate leachant This report describes activities at the experimental site, presents extensive geochemical data from startup to site restoration, compares laboratory and field experiments, and discusses the environmental aspects of acid leaching. The data showed that sulfuric acid is apparently an effective leaching solution. Three to five grams of acid per liter of ground water resulted in a production solution grade of 80 to 100 ppm uranium. Restoration was successful, but required extended flushing. The pH was the last chemical parameterto return to baseline, requiring about 350 days. This was longer than was predicted in laboratory simulations. The data also showed that mobilization of toxic elements such as selenium, arsenic, radium, thorium, and molybdenum stayed within reasonable limits and quickly fell back to preleach concentrations during restoration.

Jan 1, 1982

By L. J. Froisland

The Bureau of Mines conducted a 4-year research program at Uravan, Colo., on a 2-1/2-acre reclamation plot on the slope of a uranium tailings pile that had been covered with mine waste rock. The purpose of this study was to determine the effects of plant species, type of irrigation, type of fertilizers, and use of dust control chemicals on plant growth and surface coverage. Best grass coverage, nearly 100 percent with 240 plants per square foot, was developed in a section that was seeded with crested wheatgrass, fertilized with sewage sludge, and sprinkler irrigated. For comparison, a section that had been treated with commercial fertilizers developed 3.1 crested wheatgrass plants per square foot and 24 percent coverage without irrigation, and 8 plants per square foot and 75 percent coverage with irrigation. Results of spraying a dust control chemical were inconclusive. Russian-thistle invaded all test sections and ranged in density from 0.6 to 7.3 plants per square foot.

Jan 1, 1982

By J. S. Dunning

The Bureau of Mines investigated a series of Fe-Al-Mo alloys strengthened by ZrC (zirconium carbide) precipitates as chromium-free substitutes for stainless steels. Melting and fabrication methods were devised, and the effects of minor additions of columbium (niobium) and cerium on the mechanical properties and oxidation resistance were determined. Zirconium carbides could not be con-trolled reliably to produce fine precipitate dispersions. A more reliable carbide strengthening mechanism is required if the high-temperature strengths of types 304 and 316 stainless steels are to be duplicated. Workability and oxidation resistance of the alloy series were excellent.

Jan 1, 1982

By E. A. Johnson

The Bureau of Mines determined the effect of slag additives on copper solubility and the distribution of typical impurity elements between copper-iron matte and silica-saturated fayalite (iron silicate) slag at 1,250° C, in CO-C02 atmospheres with 10 pct S02. Small additions (<10 pct) of CaO, A1203, and MgO were shown to decrease copper solubility in the slag. Additions of CaO increased the solubility of bismuth and tellurium in the slag at lower matte grades. Al 20 3 additions decreased the solubility of tellurium in the slag, but increased that of bismuth at lower matte grades. A1203 additions increased the solubility of both at lower matte grades. With no additives, matte grade did not affect the solubility of bismuth in slags, whereas increasing matte grade resulted in a slight decrease in the tellurium solubility in slag. Additions of CaO or As203 alone to the slag increased selenium and arsenic distribution to the matte, but had little or no effect on antimony distribution; whereas small MgO additions decreased antimony distribution to the matte but had no effect on arsenic and selenium distribution. In slags with no additives, selenium distribution to the matte increased with increasing matte grade, while that of antimony decreased and that of arsenic was unchanged.

Jan 1, 1982

By D. R. Flinn

The Bureau of Mines has studied the electrochemical parameters important to the preparation of coatings of the platinum-group metals. Using molten mixtures of sodium and potassium cyanides in an inert atmosphere, techniques have been developed that permit the preparation of baths for platinum, rhodium, and iridium electrodeposition. Cyclic voltammetric and slow sweep rate linear polarization techniques have been utilized to determine optimum potential and current values for preparation of plating baths and for the electrodeposition of coatings. Techniques are described for the deposition of platinum and rhodium coatings at near 100 percent anode and cathode current efficiencies, and for iridium at approximately 80-percent efficiency. Palladium deposition from these molten cyanide baths remains un-satisfactory. The chemistry of the palladium-containing cyanide bath is discussed. Examples of scanning electron microscope photomicrographs of typical platinum coatings are presented. Techniques are described for the preparation of platinum coatings on large objects.

Jan 1, 1982

By Jerry W. Stengel

The Bureau of Mines subjected two manufacturers&apos; chemical oxygen (K02) self-rescue breathing apparatus to a series of laboratory environmental treatments designed to simulate various conditions in underground coal mines. The environmental treatments consisted of extremes of temperature, shock, and vibration. The tests were designed to be used as predictors of the ability of the self-rescuers to survive those environmental insults with no degradation in their protection to the wearer. Based on the severity of the treatments, simulating conditions more severe than offered by the mining environment, the two apparatus tested should be able to withstand the abuse offered by the mining environment and still function as intended in an emergency. Correlation of these tests with results of long-term field evaluations is needed to provide confidence in the laboratory tests as predictors.

Jan 1, 1982

By John C. Edwards

The Bureau of Mines has developed a time-dependent droplet vaporization model (in the absence of forced convection) that can be applied to the vaporization of liquid Halon 1301 droplets (vapor pressure at 300 K = 14 atm) sprayed from an extinguisher. It was found that rapid surface vaporization quickly lowers the droplets&apos; surface temperature very near to the boiling temperature, and the vaporization becomes diffusion controlled. Although the lifetime of the droplet is proportional to the square of the initial radius of the droplet, the elapsed time prior to complete droplet vaporization is not proportional to the square of the droplet radius, as an equilibrium model would indicate.

Jan 1, 1982

By V. R. Miller

The Bureau of Mines has developed a technique to separate and recover the three major components, Pb, Zn, and Cd, from lead smelter flue dust. This research was conducted as part of the Bureau&apos;s effort to reduce environmental conflicts and occupational hazards associated with mineral-processing operations and to recover valuable constituents in emissions and effluents. The laboratory process utilizes sulfation roasting of the flue dust followed by water leaching to extract over 95 pct of the cadmium and zinc. Ninety-nine percent of the cadmium was recovered from solution by cementing with zinc dust, and zinc was electrowon from the resulting solution after purification. Zinc electrolysis was carried out in a 1-liter cell at 35° C with a cathode-current density of 8 A/dm2 in a solution containing 65 g/l Zn++ and 180 g/l H2S04, Current efficiencies of 80 pct were obtained. The leached residue consisted largely of PbS04, which was converted to PbC03 and leached with H2SiF6 to produce PbSiF6 electrolyte. Ninety-five percent of the lead contained in the residue was converted to electrolyte. Lead was electrowon from solutions containing 70 gil Pb++ and 90 g/l H2SiF6 using a lead cathode, Pb02-coated titanium anodes at 28° C, and a current density of 1.6 A/dm2. Current efficiencies approaching 92 pct were obtained. Accessory minerals such as cobalt and nickel were separated into purification residues and liquor.

Jan 1, 1982

By Jacqueline H. Jansky

The Bureau of Mines conducted a study to determine the relation-ship between geologic features and linears. Cleats, kettlebottoms, and roof rolls were mapped and superimposed on the linear plots for a coal mine in West Virginia. No clear relationships were evident. This may be due, in part, to the mining practice of leaving head coal, which obscures geologic features that may exist in the roof. Future studies should concentrate on mines where roof is extensively exposed.

Jan 1, 1982

By Gary W. Kramer

The Bureau of Mines has developed a rapid analytical method for the determination of anions by ion chromatography (IC) in phosphate rock mining materials and cement kiln dust (CKD). The procedure employs an Na2C03 fusion of the sample, followed by a water extraction that allows direct injection of the sample into an ion chromatograph without separator column poisoning by the transition metal ions. Fluoride (F-) and phosphate (P043-) were determined in 24 phosphate rock processing and waste material samples by the IC method. The results were compared with a pyrohydrolytic distillation-titration method for F-and a colorimetric procedure for P043-. Excellent analytical agreement was obtained for F-and p043-values determined by IC and the comparable wet chemical methods. Fluoride values ranged from 0.3 wt-pct in the filter cake to 3.6 wt-pct in phosphate rock concentrate. Phosphate values ranged from 1.2 wt-pct in the filter cake to 33.8 wt-pct in the rock concentrate. Fluoride, chloride, phosphate, nitrate, and sulfate in several CKD samples were determined by the IC method and standard wet chemical techniques. Excellent agreement was obtained between the two methods for all anions. A total of 113 CKD samples from all areas of the United States was analyzed by the IC method. Fluoride values ranged from <0.01 to 0.36 wt-pct. Chloride values ranged from <0.01 to 12.5 wt-pct. Sulfate values ranged from 0.41 to 31.6 wt-pct. Phosphate and nitrate were detected in only about 25 pct of the samples at >0.02 wt-pct. Maximum phosphate and nitrate values were 1.0 and 1.6 wt-pct, respectively.

Jan 1, 1982

By M. M. Tilman

The Bureau of Mines conducted research to evaluate superplastic behavior in commercial magnesium-base alloys AZ6IA, ZK60A, ZW3, AZ3IB, ZWI, and an experimental Mg-12 pct Al alloy. Strain-rate sensitivity indices (m-values), maximum elongations, and effects of superplastic elongation on tensile properties were determined on fine-grained sheet. Inert-gas-pressure hemisphere-forming tests were conducted on selected sheet stock of the five alloys. Formability trials on AZ31B alloy sheet were conducted on industrial equipment for comparison with commercial superplastic forming of Zn-AI alloy. Closed-die-forming tests were performed on extruded ZK60A rod. All alloys exhibited well over 100-pct elongation, indicating superplasticity, at temperatures and strain rates near the maximum m-values. Tensile properties were generally reduced following 100-pct superplastic elongation, but not to an extent that would preclude use of the commercial alloys in the superplastically deformed condition. The potential for industrial superplastic forming of AZ31B sheet was indicated by hemisphere forming in the laboratory and substantiated in industrial forming trials.

Jan 1, 1982

By Connie S. Musulin

Radon concentrations in shallow uranium mines such as the Bureau of Mines experimental research mine are affected by barometric pressure changes. The radon concentrations show a significant correlation with absolute pressure; but over a period of days, a steady rise or fall in barometric pressure will result in noncorrelation of data. Fan shutdowns also affect radon concentrations, and an equation was derived to determine the time required for the radon concentration to return to normal after a fan shutdown, whether the ventilation is blowing or exhausting.

Jan 1, 1982

By J. C. Franklin

An experiment was conducted by the U.S. Bureau of Mines and the Canada Centre for Mineral and Energy Technology (CANMET) to measure the emanation rate of radon from cemented unclassified mill tailings in two dewatered stopes of a uranium mine at Elliot Lake, Ontario, Canada. The radon was monitored upstream and downstream and in both stopes to determine the concentration in the stopes and the amount exhausted from both stopes. The emanation rate was determined to be 0.55 pCi/cm2 sec-1 from the mill tailings, which is approximately 1,000 times higher than the average flux in the mine before backfilling.

Jan 1, 1982

By David W. Houseknecht

Probabilities of encountering coalbed discontinuities during vertical or horizontal drilling in a specific coalbed can be estimated based on analysis of mined-out areas of the coalbed where the size, shape, orientation, and distribution of discontinuities are known. The result- ant probability estimates can be applied to cost-risk evaluations of drilling programs proposed for exploratory, developmental, or methane drainage purposes in undeveloped areas of that coalbed. Data compiled from mine maps of the Beckley Coalbed in southern West Virginia were used to estimate the probabilities that discontinuities would be encountered in two illustrative hypothetical drilling programs--one for drilling vertical boreholes and the other for drilling horizontal boreholes. Analysis based on a mined-out area of the Beckley Coalbed indicated that vertical methane drainage boreholes spaced 1,000 feet apart in a square grid pattern would each have a 29 percent probability of encountering a discontinuity in a geologically unexplored area of the coalbed. It was also determined that exploratory vertical drilling could locate most of the discontinuities if a borehole spacing of 2,500 feet were used. For horizontal drainage boreholes in the Beck- ley Coalbed, the analysis indicated a linear relationship between hole length and the probability of encountering a discontinuity.

Jan 1, 1982