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By H. O. McDonald

Solutions containing Cr6+ and sulfuric acid are used in a number of surface-finishing operations. Substantial quantities of chromium and copper are lost and pollution problems are created when the spent solutions are discarded. To minimize the undesirable environmental effects while improving secondary resource recovery technology, the Bureau of Mines is conducting research to detoxify and recover metals from these solutions. Spent etchants are treated to remove copper and reduce Cr6+ to Cr 3+ in an electrolytic cell. The anodes and cathodes are granulated coke. The spent solution is continuously pumped through the electrodes. Hexavalent chromium is reduced to trivalent chromium, and copper is recovered at the cathode. Reoxidation of Cr3+ at the anode was not observed. The removal and recovery of copper reduction of Cr6+ lessen chemical demand and increase efficiency in waste in treatment operations associated with the use of these solutions.

Jan 1, 1980

By Robert P. Vinson, John C. LaScola, Fred N. Kissell, Edward D. Thimon

The face ventilation measurement method developed by the Bureau of Mines involves releasing a small volume of tracer gas (SF6) on the off-curtain side of the working face at the start of the mining cycle. At the same time, gas bottle samples are taken in the immediate return airway. The gas samples are analyzed, and a curve is drawn of SF6 concentration versus time. From this curve, the percentage of gas removed per time is calculated. A curve showing a high percentage of the tracer gas removed in a short period would represent a well-ventilated face. The face ventilation measurement method was tested in a full-scale mine entry model. Subsequently it was used underground to evaluate the spray-fan ventilation system and in an MSHA test facility to test machine-mounted scrubbers. The method was shown to be a simple and effective way of evaluating face ventilation systems.

Jan 1, 1980

By J. M. Kuchta

The chemical and thermal criteria used for predicting the spontaneous combustion hazard are briefly reviewed and data are presented to characterize the gas desorptions and self-heating tendencies of 29 U.S. coals. Closed vessel desorption experiments showed that CO, CO2, and CH4 are the main gases evolved and that the CO, CO/?O2 index, and 02 absorption rate increase with decreasing rank and increasing oxygen content of the coal. In this Bureau of Mines report, the effects of temperature, moisture, and other variables are discussed together with the application of the data to the complex conditions encountered in a mining environment. An important finding is that the presence of CO alone in a mine is not necessarily an indication of a self-heating reaction of the coal. Based upon experiments conducted in an adiabatic-type calorimeter, the self-heating temperatures of lignite and subbituminous coals can be as low as 30° C, whereas the bituminous coals require a temperature of about 60° C or more. The self-heating hazard is greatest when the coals are dried and exposed to a high humidity condition, apparently as a result of the "heat-of-wetting." Generally, the hazard is greatest with the western coals of the United States.

Jan 1, 1980

By W. H. Eddy

The Bureau of Mines used several laboratory batch flotation schemes combined with magnetic separation to investigate the feasibility of recovering potash feldspar and glass sands from molybdenite tailings. Four molybdenite tailings or prospective tailings were used as test samples. Feldspar concentrates containing from 10.7 pct to 12.0 pct K2O were recovered from three of the four samples. The alkali content of the fourth sample met the grade for a mixed feldspar. All the feldspar concentrates contained iron in excess of the 0.10-pct-Fe203 specification for most uses. Electron-beam microprobe examination of the feldspar concentrates showed the presence of an iron-bearing potash feldspar in quantities that were excessive with respect to most iron specifications. However, a high-quality glass sand was produced from all of the samples.

Jan 1, 1980

By J. A. Eisele

The Bureau of Mines conducted bench-scale cyclic tests to determine the composition of recycled leach liquor in the Bureau?s proposed clay/HCl leach/ HCl sparge process for producing Al203 from clay. The data developed from these tests make it possible to synthesize leach liquors for predetermined steady-state operating conditions when conducting large-scale crystallization tests. The results of two sparge tests were compared. One was a 20-cycle test with a 36-pct-HCl concentration in the mother liquor; the other was a 10-cycle test with a 26-pct-HCl concentration in the mother liquor. The effect of impurity concentrations in the leach liquor on the purity of aluminum chloride (AlCl30?6H20) crystals was determined, but there was poor correlation between this data and results that have been obtained from miniplant-scale work.

Jan 1, 1980

By D. Harry Chambers

The Bureau of Mines, through a memorandum of agreement with the Department of Defense, conducted research to recover silver from aircraft scrap. Silver was recovered by an electrolytic method from stainless steel honeycomb sections separated from the aircraft. These sections had been constructed by sandwiching a stainless steel honeycomb core between stainless steel sheets and then brazing the assembly with a silver alloy. Over 300 pounds of silver was used in the B-58 bomber, concentrated in certain honeycomb sections of the aircraft. Following shredding of the aircraft parts, an average of 95 percent (ranging 67 to 100 percent) of the silver was recovered in a single electro-refining step. After the electrorefined product was magnetically cleaned, purity of the recovered silver was greater than 99.3 percent.

Jan 1, 1980

By Robert F. Chaiken

A novel approach to eliminating environmental and public safety hazards that are associated with fires in abandoned coal mines and waste banks involves the use of in situ combustion technology developed by the Federal Bureau of Mines to accelerate the burning of the wasted coals in place. This technology would be used under exhaust ventilation control conditions that would allow for total management of the hot gases produced. Combustion stoichiometries would be optimized to minimize unburnt combustibles and to maximize the heat content of the gas products, which will be exhausted at one or more fan locations. When necessary, scrubber systems would be employed to remove air pollutants, such as sulfur dioxide; heat utilization systems (process heat, steam, and electricity) would also be employed to offset operational costs. Ultimately, complete burnout would solve the fire and acid water formation problems of the abandoned coal mine or waste bank. Pertinent technical data for burnout control are derived and discussed in terms of the important material and operational parameters. In general, it is believed feasible to operate a burnout system in an existing abandoned mine or waste bank fire at thermal power levels in the range of 10 to 100 Mw, and at exhaust gas temperatures of 1,000° C (1,830° F).

Jan 1, 1980

By Robert D. Schmidt

This Bureau of Mines report describes the development and application of a computer model for simulating the hydrological activity associated with in situ leaching. The model is intended to provide uranium resource developers with a description of the flow behavior of leachants and ground water during the development, production, and restoration phases of a leaching operation involving an arbitrary pattern of injection and recovery wells. Different aquifer environments are modeled, using a closed-form solution to the partial differential equation that describes three-dimensional changes in piezometric head as a result of pumping from leachant injection and recovery wells. The computer program can model a maximum of, 50 arbitarily located wells. Numerical techniques involving difference quotients and Taylor expansions about time points are used to derive time, velocity, areal sweep, and fluid volume parameters associated with leaching hydraulics. These parameters are output by the program in graphic and tabular formats. Other numeric methods insure that the program running time is minimized without significantly affect-ing the accuracy of results.

Jan 1, 1980

By R. F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Bureau of Mines has developed a general method for preparing solutions from a wide range of metal and mineral samples for chemical analysis. The development of the method from current knowledge of vessel material, pressure dissolution techniques, and the fluoride-boric acid reaction is given. The method uses 7 ml of a mixture of HC1-HNO3-HF acids in a ratio of 3.5:2:1.5 sealed in plastic bottles that act as pressure vessels when heated in a boiling water bath. A final volume of 100 ml is obtained by the addition of 93 ml of a 1. 5-pct H3BO3 solution to the bottles, which are reheated; precipitated fluorides as well as sample residue are dissolved by the fluoride-boric acid reaction. A copper slag and a steelmaking slag treated using this method were analyzed by atomic absorption spectroscopy yielding values for Si, Mg, Ca, AI, Fe, Mn, Na, As, Pb, Sb, and Zn very close to certified values with an average relative standard deviation of 2.13 pct. The low cost, reduction in preparation time, ease and safety of sample handling, conservation of reagents, and ability to dissolve volatile materials without loss make this method superior to traditional wet digestion techniques for many materials, and ideal for use with atomic absorption, and optical emission or X-ray emission spectroscopy.

Jan 1, 1980

By R. Blickensderfer

Maintaining an adequate supply of minerals and metals to meet national economic and strategic needs is the overall goal of the Bureau of Mines, U.S. Department of the Interior. One method of achieving this goal is to conserve scarce metals by cladding a plentiful base metal, such as iron, with a scarcer metal. To investigate cladding, a vacuum-rolling mill capable of rolling bimetal specimens at temperatures to 1,300° C in a residual gas pressure of 2 x 10-5 torr was established. Metals that were successfully bonded to iron included stainless steels, chromium, nickel, nickel alloys, copper, and several refractory metals including molybdenum and titanium. The effects of the rolling temperature, reduction in thickness, rolling speed, and residual air pressure on bonding strength and bend ductility of the bimetals were determined. Optimum rolling conditions produced bimetals with bond shear strength essentially equal to that of the iron base metal.

Jan 1, 1980

By H. D. Jacobs

The Bureau of Mines undertook a research program to insure an adequate supply of iron raw materials for future iron and steel making needs. A sample was obtained of oxidized taconite from the western Mesabi Range in Minnesota, and the metallurgical response of the taconite to beneficiation by a process that included selective flocculation-desliming-cationic flotation was evaluated. The sample contained 35.3 pct iron and represented approximately 2 billion tons of crude material. Selective flocculation and flotation were evaluated in a pilot plant with a feed rate of 900 Ib/hr. Concentrates averaging 61.7 pet iron and 5.1 pet silica were obtained, with an accompanying iron recovery of 67.2 pet. About 83 pct of the process water requirements were reclaimed from the slime and froth tailing and then recycled.

Jan 1, 1980

By J. E. Schiller

The Bureau of Mines has investigated the surface charge of amphibole asbestos fibers and nonasbestiform cleavage fragments, as part of the Bureau's fundamental studies to provide new knowledge on the physical and chemical properties of the amphibole minerals. Microelectrophoresis was used to measure the electrophoretic mobilities, in water, of particles from six asbesti-from amphiboles and seven nonasbestiform amphiboles over the pH range of 5 through 9. The particles generally ranged in size from 2 to 5 µm wide by 10 to 30 µm long. The isoelectric point was determined for four of the minerals, and values were found to be between pH 3.5 and pH 5. The minerals studied had zeta potentials that generally ranged from -25 to -so mv in neutral solution. Attachment of colloidal positively charged AgI was also studied as a means of determining surface charge. Scanning electron microscopy of amphibole particles that had been in contact with aqueous AgI showed equal attachment of AgI to asbestos fibers and to cleavage fragments; the extent of AgI coating was the same for both. The electrophoretic mobilities of asbestos fibers were essentially the same as those of elongated cleavage fragments of the same aspect ratio (particle length divided by width). Blocky particles from both asbestiform and nonasbestiform specimens had lower mobilities.

Jan 1, 1980

By S. A. Matthes

This Bureau of Mines report describes analysis of a copper slag for 13 elements from a single sample solution by flame atomic absorption spectroscopy. Samples are dissolved with 7 ml of an HC1-HF-HN03 (3:1.5:2) mixture in heated plastic pressure vessels. A 1.5-pct boric acid solution is added to dissolve precipitated fluorides and to reduce matrix effects that interfere with atomic absorption analysis. Preparation time is less than 1 hour per batch of 10 samples. Total analysis time is less than 6 person-hours for 130 determinations with an average relative standard deviation of 1.83 pct for the 13 elements. Simple acid standards were used for all determinations. Values obtained by this method are in excellent agreement with values obtained by slower, more costly procedures.

Jan 1, 1980

By David E. Siskind

The Bureau of Mines studied airblast from surface mining to assess its damage and annoyance potential, and to determine safe levels and appropriate measurement techniques. Research results obtained from direct measurements of airblast-produced structure responses, damage, and analysis of instrument characteristics were combined with studies of sonic booms and human response to transient overpressures. Safe levels of airblast were found to be 134 dBL (0.1 Hz), 133 dBL (2 Hz), 129 dBL (6 Hz), and 105 dB C-slow. These four air-blast levels and measurement methods are equivalent in terms of structure response, and anyone could be used as a safe-level criterion. Of the four methods, only the 0.1-Hz high-pass linear method accurately measures the total airblast energy present; however, the other three were found to adequately quantify the structure response and also represent techniques that are readily available to industry. Where a single airblast measuring system must he used, the 2-Hz linear peak response is the best overall compromise. The human response and annoyance problem from airblast is probably caused primarily by wall rattling and the resulting secondary noises. Although these will not entirely be precluded by the recommended levels, they are low enough to preclude damage to residential structures and any possible human injury over the long term.

Jan 1, 1980

By Seth C. Schaefer

[As part of the Bureau of Mines effort to provide thermodynamic data for advancement of mineral resources technology, the standard Gibbs energies of formation (?G°f) of MnS (manganese sulfide) and Fe0.9 S (pyrrhotite) were investigated with a high-temperature galvanic cell employing stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, MnS, MnO, S02 (g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt with the overall cell reaction MnS (s) + 1.5 02 (g, 0.0114 atm) = MnO (s) + S02 (g) . (1) These results give the standard Gibbs energy of formation of MnS for the reaction Mn (s) + 0.552 (g) = MnS (s) (2) ?G°f = -66.487 + 15.19 x 10-3T±0.207 kcal/mole (896.4 - 1,208.1 K) (3) where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, FeO .9S, Fe304 , S02 (g, 1 atm) //Zr02//02 (g, 0.0114 atm) , Pt with the overall cell reaction 10/3 FeO .9 S (s) + 16/3 02 (g, 0.0114 atm) = Fe.,04 (s) +10/3 S02 (g). (4) These results yield the standard Gibbs energy of formation for the reaction 0.9 Fe (s) + 0.5 S2 (g) = Fe0.9 S (s) (5) ?G°f = -35.229 + 12.67 x 1073T+-0.104 kcal/mole (839.5 - 1,086.6 K). (6) A third-law analysis of MnS data yields a standard enthalpy of formation (AH°f) for the reaction Mn (s) + S (rh) = MnS (s) (7) ?H°f298 = -51.16±0.21 kcal/mole (8) A similar third-law analysis for Fe0.9S data yields a ?29°f298 for the reaction 0.9 Fe(s) + S(rh) = FeO .9S(s) (9) ?HO\°f298 = -24.01±_0.15 kcal/mole. (10) ]

Jan 1, 1980

By James H. Russell

The Bureau of Mines, U.S. Department of the Interior, in cooperation with the Department of Energy, has attempted to increase the activity of nickel catalysts for converting synthesis gas, derived from coal, to a substitute natural gas. This report describes the effects of low-level additions of B, Ca, Ce, Co, Mn, Mo, Pd, Re, Ti, Y, Zn, and Zr on the methanation activity of Raney nickel. The methanation rate at 320° C and the resistance to poisoning by 2 ppm H2S were used to compare catalysts. The effects of the additions were small, and the experimental variances were large, necessitating the use of statistical methods to identify significant effects. Co, Ti, Y, and Zn improved the resistance to H2S poisoning, but only Co improved the methanation rate In some individual catalysts containing Ca, Mo, or Mn, both the methanation rate and resistance to H2S poisoning were improved.

Jan 1, 1980

By V. R. Spironello

The Bureau of Mines is involved in research directed toward the conserva¬tion of important raw materials and the utilization of solid waste. Two of the objectives are to conserve high-quality coking coals used for foundry coke and to utilize waste materials of marginal quality but of high calorific value. These objectives are consistent with Bureau goals. Pilot plant cupola trials were made to evaluate the adequacy of various alternative fuels, and to determine to what extent they could replace the foundry coke in cupola charges. Information was obtained on furnace performance, metal and slag chemistry, environmental questions, and the properties of castings. It was shown that anthracite or bituminous coals can partially replace charge coke up to the 40 pet level. Briquetted materials prepared from fuel fines, and waste prod¬ucts or byproducts of high calorific value, all tend to break down on heating in a cupola so that their use must be restricted to below 20 pet replacement. In cases where pitch-bonded coal fines or petroleum coke were used, carbon pickup by the iron was inadequate for gray iron specifications. Although emphasis during this work was placed on basic slag practice, some acid practice results are included.

Jan 1, 1980

In Bureau of Mines research on recycling chrome refractory wastes, used refractories from argon-oxygen decarburization and electric steelmaking furnaces were beneficiated, concentrates were reformed into briquets, and modulus of rupture tests were conducted at 1,350° C. The test results indicated that the beneficiated minus 6-mesh material could be used for producing magnesia-chrome refractories.

Jan 1, 1980

By Jon K. Ahlness

The Bureau of Mines, in cooperation with the Institute of Mineral Research of Michigan Technological University, and the Upper Great Lakes Regional Commission, conducted an investigation of electronic sorting of native copper ore from Upper Michigan. This report is based on research by the Institute of Mineral Research under contract to the Bureau. The test program evaluated the use of belt and rotary sorters on various size and grade fractions of ore. Both plant-scale sorting and lab sorting tests were run. The plant sorting objectives were to determine the sortability of different ores and the efficiency of the electronic ore sorters. High-and low-grade ores from both conglomerate and amygdaloid types were separated into four size fractions. The two larger sizes were sorted on belt sorters and the two smaller ones on rotary sorters. Copper recoveries ranged from 20.0 pct from a feed grade of 0.40 pct to 80.3 pct from a feed grade of 1.08 pct. Lab sorting tests of conglomerate ore were run to determine the efficiency of a belt sorter equipped with a second sensing coil located above the belt and to determine the sorting characteristics of larger ore size fractions than those used in the plant sorting. Copper recoveries from the combined feed sizes ranged from 47.0 pct from a feed grade of 0.13 pct to 96.8 pct from a feed grade of 4.87 pct. For all the ore types except one, it was found that the copper recovery increased with the feed size.

Jan 1, 1980

By K. Robert Dorman

This Bureau of Mines report describes laboratory and field experimentation in building mine ventilation stoppings, air-door frames, and fan bulkheads with a civil construction technique. Shotcrete is applied to a free-standing, three-dimensional wire-truss panel, which is easily cut and rapidly erected. In mines where shotcrete equipment is available, this technique should be faster and cheaper than conventional block-and-mortar or monolithic concrete construction.

Jan 1, 1980