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By Robert Lee Stahl

Comprehensive field tests were made by the Federal Bureau of Hines at the Conda open pit mine near Soda Springs, Idaho, to determine whether surface geophysical techniques could be used to detect and delineate faults in phosphate deposits. The tests included seismic refraction, magnetometry, electrical resistivity, and airborne photography. Of the several geophysical techniques tested in the field, horizontal resistivity profiling was the most effective method for diagnosing faults. The method is quick, inexpensive, accurate, and can be easily used by mining company personnel to detect and delineate faults.

Jan 1, 1975

By Michael L. Boucher

Copper and nickel sulfides occurring in the Duluth Complex of northern Minnesota were examined at the Bureau of Mines, A microscopic study was undertaken to determine the mineralogy and paragenesis of the ore minerals. Eighty-two samples were taken from one deep diamond drill core located near Babbitt, Minn. Modal analyses are presented for the Duluth Complex rocks and for the are minerals in the major mineralized zone. The major sulfide minerals are chalcopyrite, cubanite, pyrrhotite, troilite, and pentlandite. Results of this investigation suggest that the mineralization is related to the structural features of the enclosing rocks: pores, open fractures, and cavities. The pyrrhotite-troilite-pentlandite assemblage is believed to have formed from an immiscible sulfide melt, probably associated with the troctolitic rocks. Most of it settled to the very porous base of the Duluth Complex, and to the other porous zones near xenoliths; small portions were trapped higher in the section. A later introduction of a copper-rich sulfide melt replaced some of the pyrrhotite-troilite and oxides, and filled in the remaining open spaces and fractures in the Duluth Complex and those of the adjacent footwall rock.

Jan 1, 1975

By Jack C. White

The purpose of this Bureau of Mines research was to determine the technical feasibility of direct sulfuric acid digestion of Florida land-pebble phosphate matrix. Preliminary tests in a continuous digestion circuit showed that 92 to 96 percent of the P2O5 contained in the matrix was extracted, while the P.05 concentration in the product acid ranged from 21 to 30 percent. The waste filter cake contained about 1 percent P205 and up to 18 percent water. These sandy compact filter cakes, comprised mostly of quartz and gypsum, appeared to be suitable for backfilling and reclamation of mined lands.

Jan 1, 1975

By D. D. Fischer

Recovery and separation of molybdenum and rhenium from a process solution was accomplished by a technique developed by the Federal Bureau of Mines involving a combined solvent extraction and activated carbon adsorption procedure. The processing sequence required treatment of the solution with S02 to reduce the chlorate ion and adjust the pR prior to solvent extraction of molybdenum and rhenium with a tertiary amine. Molybdenum and rhenium were stripped from the organic phase with an NH40H solution, and the strip solution was then passed through activated carbon to preferentially adsorb the rhenium. After washing entrained molybdenum from the column with a brine solution, rhenium was eluted with an MeOH-H20 mixture. The activated carbon was regenerated with water. Molybdenum was recovered as (NH4)6Mo7024 by evaporating the column effluent. Rhenium in the column eluate was reextracted with a tertiary amine, stripped from the organic phase with dilute NH40H, and recovered as NH4Re04 by evaporating the strip solution. The final (NR4)Re04 product contained < 80 ppm impurities. Sodium sulfate was crystallized from the first solvent-extraction raffinate by lowering the solution temperature to 0° C. Precious metals contained in the original process solution were adsorbed onto the activated carbon.

Jan 1, 1975

By Seth C. Schaefer

The Bureau of Mines studied the standard free energies2 of formation of ferrous fluoride (FeF2) and ferric fluoride (FeF3) with high-temperature galvanic cells employing calcium fluoride doped with 1 mole-pet yttrium fluoride as the electrolyte. A free-energy change for the cell reaction Fe (s) + NiF2 (S) = FeF2 (S) + Ni (s) together with the standard free energy of formation of nickel fluoride yields a standard free energy of formation of ferrous fluoride from the elements of ?GF° = -168.74 + 30.63 x 10-3T ± 0.41 kcal/mole (897-1,098 K). (2) Combining the standard free energies of formation of magnesium fluoride, ferric oxide, and magnesium oxide with the free-energy change for the overall cell reaction 3MgO(s) + 2FeF3 (s) = 3MgF2 (S) + Fe2 03 (S) (3) gives a standard free energy of formation of ferric fluoride from the elements as ?Gf° = -281.45 + 90.46 X 10-3T ± 0,67 kcal/mole (880-935 K). (4) Free energies and equilibrium fluorine pressures for the two univariant equilibria of the Fe-F system are tabulated and illustrated.

Jan 1, 1975

By S. R. Borrowman

Mill tailings from conventional uranium extraction processes contain nearly all of the radium originally in the ore. Such tailings require controlled storage in perpetuity to safeguard the surrounding environment from radioactive contamination. Alternatives to controlled storage of the tailings are (1) removal of the radium from the tailings for separate storage or use or (2) removal of the radium when processing the uranium ore. In laboratory tests conducted by the Federal Bureau of Mines, radium was leached from tailings using either hydrochloric acid or ethylenediamine tetraacetic acid. A hydrochloric acid leaching method was used to extract both radium and uranium from the ore to yield tailings containing less radium than those produced by either conventional sulfuric acid or alkaline leaching processes. From 77 to 94 percent of the radium in mill tailings was concentrated by sedimentation in slime fractions representing nearly 25 weight-percent of the original sample.

Jan 1, 1975

By R. A. Guidotti

The Federal Bureau of Mines studied the thermal decomposition of the nitrides of the Group V A metals (CbN, Ta3N5, and VN) with the goal of preparing high-purity metals. Solid-state purification and arc and electron-beam melting were examined. Electron-beam melting proved to be the most efficient means of nitrogen and oxygen removal. Columbium and tantalum of 99.9-pct purity were prepared by this technique; in the case of vanadium, however, nitrogen could not be reduced below the solid-solution level.

Jan 1, 1976

By Carl F. Wingquist

Electrical resistance heating to effect thermal fragmentation of semiconductive rock was examined by the Bureau of Mines. Tests were carried out on copper-bearing ores of the Nonesuch Shale Formation in the laboratory and in the the field at White Pine, Mich. Fieldwork included primary and secondary breakage tests. Heating tests on in situ rock failed to produce thermal dam-age to an extent considered useful; however, boulders up to 30 ft3 were effectively broken by the method. Power input to the test rock was taken from a 50-kV, 5-amp dc power supply.

Jan 1, 1976

By E. E. Maust

The literature on the activation of sphalerite for flotation by short¬chain xanthates leaves unanswered the question of whether a compact surface film of activator sulfide is necessary or merely sufficient for high flotation recoveries. Studies by Guarnaschelli and Plaksin indicate that xanthate adsorption and flotation of sphalerite are increased with increasing hole/ electron ratio. These results, and the known acceptorlike behavior of many heavy-metal impurities in zinc sulfide, suggest that activation may result from a traditional semiconductor doping effect at the surface. Using the theory of chemisorption states on ionic crystals as developed by Levine and Mark, the Bureau of Mines has carried out A calculation to estimate the surface-state energies of various metals when they are substituted at zinc sites on (110) sphalerite surfaces. Based on a simple Madelung-Born treatment of ionic solids, the calculation indicates that many of the metals known to activate sphalerite for subsequent flotation have lower surface-state energies than nonactivators. The results of these calculations are discussed from the standpoint of consistency with the proposed activation mechanism and observed flotation results. The satisfactory agreement obtained is taken to be support for the proposed mechanism, and further elaboration of a surface-doping model is attempted.

Jan 1, 1976

By K. C. Dean

Time and motion studies were made by the Federal Bureau of Mines on the hand and machine dismantling of scrapped auto starter motors, generators, and alternators for recovery of copper, aluminum, and iron. The studies showed that an individual with power handtools and convenient access to a hydraulic press, power bandsaw, acetylene torch, and power lathe could, in an 8-hour day, disassemble about 100 starters, or 150 generators, or 30 alternators. The scrap copper yield would be 280, 390, and 45 pounds, respectively, and the iron yield would be about seven times the copper weight. About 100 pounds of aluminum would be obtained from the alternators.

Jan 1, 1976

By L. W. Higley

Electrowinning metals from solutions leached from low-grade ores is becoming an increasingly important extraction method as the metal industry turns to pollution-free recovery processes. Lead-alloy anodes are used industrially in the electrolytic recovery of zinc and copper. However, associated with the use of these anodes are the inherent problems of stability and lead contamination of the cathode. In an effort to eliminate these problems, the Bureau of Mines has developed a relatively inexpensive lead dioxide anode for electrowinning metals from strong acid solutions. The anode was prepared by depositing Pb02 directly on a titanium blank in a strong HN03-Pb(N03)2 solution at 2.15 to 6.45 A/dm2 and 60° C. This anode was tested in zinc and copper electrowinning cells containing 200 gpl H2S04 and 35 to 100 gpl metal ions at the current density of 3.23 to 6.45 A/dm2. Contamination of the cathode by lead was =0.005 pet. A 30-day test at 6.45 to 12.90 A/dm2 in an electrolyte containing 200 gpl H2S04 and no metal ions resulted in a slight change in surface morphology of the Pb02 anode but no measurable change in anode weight or dimensions.

Jan 1, 1976

By Philip E. Sanker

The Bureau of Mines conducted small-scale batch and semicontinuous tests on the reduction of zinc sulfide with iron according to the reaction ZnS + Fe ? FeS + Zn to determine reaction kinetics in the temperature range 1,000° to 1,400° C and to investigate the potential use of a scrap iron reductant. Batch tests indicated that a temperature of at least 1,300° C with a 1:1 mole ratio of Fe to ZnS is needed for good zinc recovery. Semicontinuous tests were conducted, using four zinc concentrate samples, containing various percentages of copper, cadmium, and lead, which were reacted with iron and iron contaminated with iron oxide and tin in an externally heated graphite furnace. Analysis of the zinc metal and FeS matte reaction products showed cadmium to be entirely in the zinc metal, copper to be in the FeS matte, and lead to be about 60 pct in the zinc metal and 40 pct in the matte. Tin reported to the matte, and none was detected above the O.OS-pct level in the zinc. Sulfur dioxide was not detected in the offgas when up to 20 pct of the iron was replaced by Fe203.

Jan 1, 1976

By J. B. Janus

This report, the 25th in a series, lists analytical data of coal samples collected by the Bureau of Mines in connection with the purchase of several million tons of coal for various Government agencies during fiscal year 1975. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for these coalbeds only. The delivered coal was sampled at destination in accordance with instructions furnished by the Bureau of Mines, and all samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1976

By D. A. Wilson

A laboratory method for processing lead battery scrap has been developed that eliminates virtually all of the S02 emission that normally is produced when a reverberatory or blast furnace is used. The method employs a hydrometallurgical step to convert the PbS04 to PbO and CaS04 by mixing the battery scrap with a slurry of Ca(OH)2. The reaction is exothermic and goes to completion in 2 to 5 minutes at room temperature. The dried product is mixed with a KC1-NaC1 flux and carbon and reduced at 6500 C. A minimum charge ratio of 3 parts of carbon to 100 parts of battery scrap is required for reduction. The process produces lead reductions and recoveries as high as 97.0 and 94.9 percent, respectively. The KCI-NaCl flux is recovered using a standard counter-current water leach followed by evaporation.

Jan 1, 1976

By Martin Hertzberg

The concept of limit burning velocities is used to formulate a quantitative theory of flammability limits. Competing processes dissipate power from a combustion wave and quench propagation at some characteristically low limit velocity. There are four competing processes and one complication: (a) Free, buoyant convection, (b) conductive-convective wall losses, (c) radiation, (d) selective, diffusional demixing (the complication), and (e) flow gradient effects (flame stretch). These complexities are unraveled by creating an idealization that is initially freed from these competing processes. The ideal serves as a standard, and its burning velocity (Su), ideal is a unique function of the initial thermodynamic variables of state. By adding each process individually, it is possible to evaluate their significance, quantitatively, in terms of a limit velocity (Su)a , b , c , or e , and to explore the nature of their cooperative interactions. The larger the limit velocity, the more significant the process. The apparently diverse observations of flammability behavior are readily unified within this simple, conceptual framework.

Jan 1, 1976

By D. L. Paulson

The Bureau of Mines is investigating pyrometallurgical and chemical methods for extracting copper from sulfide ores under conditions that provide for control of gaseous and solid emissions. Under this program, a new electrothermic reduction process was developed to produce blister copper after collecting essentially all of the sulfur by a single-unit operation. The process feasibility was indicated by a laboratory-scale investigation that demonstrated chalcopyrite concentrate can be roasted to less than 1 percent sulfur and that the resulting calcine can be reduced with carbon to blister copper by a cyclic process in a single arc-smelting furnace. Pilot-scale tests in an 800-kV-A electric-arc furnace demonstrated that 98.4 pct of the contained copper can be continuously recovered as metal by operating at bath temperatures between 1,350° and 1,375° C. Smelting rates of approximately 225 lb of blend ft2 of bath surface/hr resulted in power consumptions of approximately 520 kW-hr/ton of blend. The blister copper that was produced contained less than 0.1 pct iron while the precious metals reporting to the copper product and gangue material elimination were similar to those in a conventional smelting operation.

Jan 1, 1976

By P. W. Jerant

The methane emissions from an advancing coal mine section were continuously monitored for 120 days. During this time, the section advanced 2,000 feet into virgin Pittsburgh coalbed producing 54,565 tons of coal with a total methane emission of 91 million ft3. Analysis of the data gathered showed that daily methane emissions did not correlate with overburden thickness and daily coal production. A good correlation was found between the daily methane emission and the average length of rib exposed to virgin coal.

Jan 1, 1976

By Maria I. De Rosa

High temperatures encountered by mine rescue teams during emergency situations may cause severe physiological strain, hindering the men from carrying out rescue and recovery missions. A prototype ice-cooling garment (ICG) was developed by the Bureau of Mines to alleviate physiological strain due to heat stress. The effectiveness of the garment was tested with acclimatized and unacclimatized subjects at a typical work rate (1,200 Btu/hr) expected during rescue operations and at various hot environments (97° to 113° F dry bulb and 80° to 89° F wet bulb). During exposures with the ice cooling garment, the subjects were able to maintain a safe deep body temperature of 100.4° F or below Without the garment, the deep body temperature rose beyond values of 100.4° F, a condition considered unsafe for continuous work in hot conditions. Both heart rate and skin temperature values were lower while wearing the ICG. Subjective observation also indicated a marked benefit by wearing the ICG.

Jan 1, 1976

By G. W. Elger

This report describes pilot-plant studies and an economic evaluation of a process developed by the Federal Bureau of Mines, Albany Metallurgy Research Center, to produce synthetic rutile from a rock-type ilmenite concentrate. In this process, ilmenite blended with coke and lime is smelted in an electric arc furnace to separate most of the iron as salable pig iron and to form a titania-enriched slag of low iron content, which is treated with oxygen and titanium pyrophosphate. The titanium oxides are converted to crystalline rutile; the phosphate glass contains most of the associated impurities. The treated slag is ground and leached with sulfuric acid to liberate rutile crystals, which are concentrated by physical methods. In pilot testing conducted to obtain data for a cost estimation, a synthesized product containing about 88 wt-pct TiO2 and less than 2 pct FeO was extracted from a rock-type ilmenite concentrate containing about 45 wt-pct TiO2. The estimated fixed capital cost (on a mid-1975 basis) of a plant producing 500 tpd of synthetic rutile is $28,290,100. Based on 330 operating days per year, the estimated operating cost for this process is $351 per ton of synthetic rutile. The estimated selling price of synthetic rutile made from rock-type ilmenite is $344 per ton, based on a credit of $160 per ton of pig iron and a 20 pct interest rate of return on investment after taxes.

Jan 1, 1976

By E. E. Maust

The present work is part of an ongoing Bureau of Mines effort to provide a better understanding of the fundamental phenomena involved in sulfide flotation, the role of oxygen in xanthate adsorption being one essential issue. Galena was chosen as the material around which to develop a conceptual model, partly because of its demonstrated oxygen sensitivity and partly because information on its properties and flotation behavior constitutes the largest part of the fundamental information available on sulfides of commercial importance. The model is formulated primarily in terms of surface electronic energy levels produced by oxygen and xanthate and is further developed using existing experimental evidence and its implications. Four major functions of oxygen are elucidated, and the relationship of these to the formation of lead xanthate, dixanthogen, and a surface compound is discussed. Though yet incomplete, the model provides a useful framework within which the results of diverse experiments can be related to one another in their proper perspective, as shown by a brief discussion and resolution of some apparently discordant results reported in the literature.

Jan 1, 1976