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By Robert W. Freedman

This report describes sampling and analytical procedures used for measurement of sulfates in diesel tailpipes and in the diluted exhaust within dilution tunnels. A variety of methods exist for sulfate analysis for such systems, including ion exchange. Two chemical methods used by the Bureau of Mines are described in detail. These are based upon spectrophotometric measurement of chloranilic acid using barium chloranilate. The procedures are rapid and relatively inexpensive. In general, ion exchange is preferred by many analysts for sulfate analysis. However, it is more complex and expensive than chloranilic acid procedures, which are adequate for exhaust analysis.

Jan 1, 1982

By T. J. Driscoll

Methane-air mixtures can ignite as a result of sparking or rubbing of materials, particularly by impact involving light alloys and rusted steel where an exothermic thermite reaction can occur. This report reviews the published literature and describes a new method utilized by the Bureau of Mines for studying the processes occurring during collisions of light metals with rusted steels. The method involves measuring the spectra of sparks and explosions in methane-air mixtures using a photodiode array. Initial results obtained using magnesium and aluminum alloy 6061-T651 projectiles striking rusted steel are reported. These results indicate that the continuous parts of the spectra show a larger intensity for incendive sparks compared with nonincendive sparks, with the largest relative change in the higher energy, ultraviolet region. An unexpected shift of the intensity maximum for the continuous parts of the spectra towards the infrared region was observed for the more incendive sparks. Evaluation of rusted steel samples with electron microscopy, energy-dispersive X-ray spectrography, and Auger electron spectroscopy after they had been impacted by aluminum alloys indicated that aluminum was transferred to the steel in the form of islands that became larger as a function of increasing projectile velocity.

Jan 1, 1982

By Arthur V. Petty

In Bureau of Mines research on recycling chrome-containing refractory wastes, used refractories from argon-oxygen decarburization and electric steelmaking furnaces were beneficiated. By means of dry magnetic separation on minus 6-mesh crushed wastes, a concentrate was produced. After minor adjustments to the particle size distribution, full-size refractory brick were dry-pressed by a commercial producer and fired to 1,450° and 1,730° C. Standard testing procedures were used to determine the cold-crushing strength, modulus of rupture at 25°, 1,300°, and 1,500° C, hot load, thermal shock resistance, thermal expansion, and slag resistance. Optical and electron microscopy were used to determine grain-bonding mechanisms, and energy-dispersive analysis of X-rays was used to determine elemental distribution. The test results indicate that the beneficiated material could be used to produce a refractory product suitable for moderate-temperature applications.

Jan 1, 1982

By R. O. Dannenberg

The Bureau of Mines conducted laboratory batch and small-scale continuous tests to remove traces of dissolved molybdenum from water simulating waste discharged from a molybdenum concentrator, Molybdenum concentrations, initially ranging from 2 to 10 ppm, were decreased to 0.5 ppm or less by coprecipitation of the molybdenum with freshly precipitated ferric hydroxide" The precipitate was separated as a froth by dissolved-air flotation for subsequent disposal. Although the treated water met current environmental standards for contained molybdenum, contained particulate iron might have to be removed by filtration for the water to be acceptable. Estimated costs for treating concentrator effluent water were 55 cents, 57 cents, and 64 cents per 1,000 gal at initial molybdenum concentrations of 2, 4, and 10 ppm, respectively.

Jan 1, 1982

By J. I. Paige

As part of a continuing effort to develop technology that maximizes mineral and metal recovery from domestic resources, the Bureau of Mines investigated a method to totally utilize copper converter slags without recycling them back through the matte smelting furnace. The research was directed toward (1) recovering the contained copper in converting slags by producing a recyclable copper-iron matte, (2) carbothermically reducing the slags to recover the iron, and (3) producing slag wool from the depleted slags. This report deals with the reduction of three industrial converting slags, containing 2.0 to 7.3 wt-pct Cu, in an 800-kVA electric arc furnace to produce a recyclable copper-iron matte. The addition of sufficient iron pyrite to provide 29 to 113 pct of the stoichiometric sulfur (based on producing 40-pct-Cu matte) produced a recyclable matte (36 to 61 pct Cu) at an energy consumption of 520 to 700 kWh per ton of solid material charged. The expected energy saving for treating molten slag in an electric furnace (5-to 9-MVA range) is about 400 kWh per ton of molten slag treated.

Jan 1, 1982

By H. C. Ko

As part of the Bureau of Mines effort to provide thermodynamic data for the advancement of mineral technology, the standard enthalpies of formation for ZnO?2ZnSO4 and COS04-6H20 were determined by HC1 acid solution calorimetry. The values are -550.31 ±0.28 and -641.33 ±0.15 kcal/mot, respectively.

Jan 1, 1982

By E. Morrice

As part of its efforts to maximize process efficiency and decrease energy requirements in mineral processes, the Federal Bureau of Mines has investigated methods for beneficiating bastnäsite ores from Mountain Pass, Calif. The results of a bench-scale study on the flotation of bastnäsite ore are presented. Flotation at a pulp temperature of 40° to 45°C yielded a cleaner concentrate containing 58.7 pct RE203 at a rare-earth recovery of 67 pct. These results are comparable to those reported for the commercial beneficiation method in which the pulp is heated to boiling before flotation. An attempt was also made to recover a barite flotation concentrate from the bastnäsite rougher tailing. Concentrates containing only 70 pct barite were obtained.

Jan 1, 1982

By H. H. Dewing

The Bureau of Mines constructed a process research unit (PRU) to demonstrate new technology for extracting zinc from sphalerite concentrates. Up to 9 kg/hr of sphalerite (ZnS) concentrate was reacted at ambient pressure in the PRU with 80 pct sulfuric acid at 160° to 180° C to produce zinc sulfate and elemental sulfur. The PRU consisted of a three-stage glass reactor system: a 4-liter premix stage in which feed was slurried with 78 to 82 pct H2S04, a 40-liter stirred reactor, and a ISO-liter settling stage in which high reaction conversions were effected and excess H2S04 for recycle was separated from insoluble ZnS04 and sulfur. Evolution of sulfur-containing gases was minimized by sub-surface addition of acid feed slurry to the stirred reactor and by exclusion of air from the reactor to prevent the oxidation of elemental sulfur. Conversion of zinc to zinc sulfate averaged over 99 pct at the optimum acid concentration of 80 pct. Total sulfur losses (primarily S02) were less than 2 pct of the sulfur in the sphalerite. Elemental sulfur remained in the insoluble portion of the settled reactor product after leaching with simulated spent zinc electrolyte containing sulfuric acid. The sulfur residue contained 75 to 89 pct sulfur. Neutral zinc sulfate, required for zinc electrowinning processes, was separated from the sulfuric acid leach solution by crystallization at -15° C as zinc sulfate heptahydrate (ZnS04?7H20). The crystallization operation simultaneously effected a partial concentration of the recycled electrolyte solution by removing water.

Jan 1, 1982

By John P. Coughlin

Software techniques developed by the Bureau of Mines Denver Research Center for real-time microseismic data analysis are presented. These techniques focus on the simple acquisition of P-wave arrival times and their use in event location. The paper discusses in detail software techniques to separate microseismic events from mining noise such as drilling and from very large events such as rock bursts. Incorporation of these techniques has enhanced the reliability and accuracy of computer-based monitoring of microseismic activity in ongoing research by the Bureau.

Jan 1, 1982

By Francis R. Redfern

Newton's method of solving a nonlinear equation is employed to develop a least-squares acoustic emission source location method in which the spatial residuals of the location equations are minimized. These residuals, related to the distances from the least-squares source location perpendicular to the surfaces described by the location equations, permit location error to be estimated to first order along the spatial axes. The solutions obtained by this method are the best spatial solutions to the location equations in the least-squares sense. Also presented is a procedure by which the geometrical control of a transducer array can be evaluated using the rate of change of source location with fractional velocity change.

Jan 1, 1982

By J. W. Walkiewicz

One of the objectives of the Bureau of Mines is to develop substitution technology for scarce materials. In accordance with this goal, alloys containing lanthanum, cobalt, copper, and magnesium were investigated for fabrication of rare-earth-cobalt (RE-Co) permanent magnets. A complete substitution of lanthanum for samarium and a partial substitution of copper for cobalt was accomplished. Magnets of La-Co and La-Co-Cu-Mg alloys were fabricated by powder metallurgy techniques and evaluated. A maximum intrinsic coercivity of 23.2 kOe was obtained with a La-Co-Cu-Mg alloy. In comparison, maximum values of 9.3 kOe and 11.6 kOe were obtained with La-Co and La-Co-Cu alloys, respectively. The substitution of copper and magnesium for part of the cobalt resulted in a large increase of intrinsic coercivity, similar to the results of Bureau research with mischmetal-Co-Cu-Mg alloys. Unlike the mischmetal-Co-Cu-Mg magnets, the La-Co-Cu-Mg magnets showed signs of physical deterioration on exposure to air. The effects of fabrication parameters on the magnetic properties of the La-Co-Cu-Mg alloys were also determined.

Jan 1, 1982

By P. R. Bremner

The United States is more than 90 pct dependent on imported bauxite a source for aluminum, but it has vast nonbauxitic aluminum resources, such as kaolinite, anorthosite, alunite, etc. As part of a program to devise processes for treating these resources, the Bureau of Mines investigated a bench-scale leaching process using hydrochloric acid (HC1) and fluoride to extract aluminum from Wyoming anorthosite. HC1 and fluoride-to-aluminum (F/Al) mole ratios were studied with respect to aluminum extraction for single-stage, cocurrent, and countercurrent leaching modes. Using 95 pct stoichiometric HC1 and a F/Al mole ratio of 0.27, 90 pct of the aluminum was extracted by countercurrent leaching. Single-stage leaching with the same amount of acid and fluoride extracted 48 pct of the aluminum. Three fluoride sources, CaF2, Na2SiF6, and H2SiF6, were used and gave similar results on aluminum extractions.

Jan 1, 1982

By J. H. Russell

As part of its efforts to maximize resource recovery, the Bureau of Mines conducted studies to recover valuable byproducts from Western phosphate beneficiation tailings. Potential byproducts include phosphorus, vanadium, and uranium. The objective was to determine roasting and leaching conditions for maximum dissolution of vanadium from tailings containing approximately 13 pct P205 and 0.23 pct V. Sulfuric acid leaching tests were conducted with the tailings either as a dilute suspension dried, or in a roasted condition with or without NaCl added during roasting. More than 90 pct of the vanadium was dissolved by roasting at 850° C for 120 min with 8-pct NaCl and leaching at 75°C for 120 min with an excess of 2N H2S04, By roasting without NaCl and avoiding the difficulties of the chloride impurity, nearly 80-pct vanadium dissolution was achieved with an 800° C roast for 180 min. Quadratic regression equations were derived to relate vanadium dissolution to roasting and leaching conditions.

Jan 1, 1982

By A. D. Mah

To assist Bureau of Mines research in extractive metallurgy and to add to the thermodynamic data base useful to others, energy calculations were made for 63 reactions relating to investigations on the production of anhydrous aluminum chloride from chlorination of clay.

Jan 1, 1982

By J. I. Paige

The Bureau of Mines, U.S. Department of the Interior, conducts research on methods to minimize the requirements for mineral raw materials through conservation, substitution, and increased minerals and metals recovery from primary and secondary domestic resources. To further this goal, prior Bureau research had devised a pyrometallurgical technique (RI 8211) to recover metallic iron and copper from molten copper smelting furnace slags by carbothermic reduction. As a continuation of this Bureau research on the carbon injection technique, reverberatory and electric furnace slags were treated in an 800-kva electric arc furnace by simultaneously top feeding the slag and injecting coke breeze into the bottom of the molten bath. Results of the tests show that 76 to 89 pct of the copper and up to 48 pct of the iron contained in the smelting furnace slag were recovered in a metallic phase, while 56 to 82 pct of the carbon injected into the sys-tem was utilized as the reductant. Laboratory evaluation has shown that the metal product, which contains 86.9 to 95.0 wt-pct iron and 1.3 to 4.1 wt-pct copper, will be a satisfactory medium for recovering copper by cementation. The expected energy consumption for the process is 110 kwhr per ton of molten slag treated and 520 kwhr per ton of solid material charged.

Jan 1, 1982

By William H. Pomroy

The Bureau of Mines, through a 4-year program of combined in-house and contract research, has developed the necessary hardware and software technology to provide rugged, reliable automatic fire protection for surface mining mobile equipment. One element of this program was a continuing effort to help foster rapid mining industry acceptance of the technology by keeping end user costs reasonable. This report is an analysis of the economic impact of surface mining mobile equipment fires and the cost benefit of utilizing automatic fire protection systems to abate these losses.

Jan 1, 1982

By Victor R. Spironello

The Bureau of Mines has conducted studies of the slags related to ferrous technology to evaluate experimentally acceptable substitutes for the auxiliary flux, mineral fluorspar, in steelmaking operations. Comparative heats were made in a 1/4-ton, pilot-scale, basic oxygen furnace (BOF) to evaluate a waste material known as "used potlining." Used pot lining is recovered from alumina reduction cells after its useful life and contains significant levels of fluorine and sodium in various compounds. This material in both lump and pelletized form provided adequately fluid slags, based on observations made during BOF operation. No adverse effects were found on furnace performance, metal and slag chemsitry, the strength of the steel produced, or the environment. Fluorine recovery in the slag was about the same as that obtained when using fluorspar, as were the losses to the scrubber water and solids. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag. The sodium recovered in the slag apparently also contributed to fluidity, since the fluorine input was at about two-thirds that of the fluorspar. Used potlining was determined experimentally to be a satisfactory substitute for fluorspar in basic oxygen steelmaking.

Jan 1, 1982

By David M. Hyman

The Bureau of Mines has developed two experimental designs for deter- mining the volumes and relative proportions of the various gas species, particularly methane (CH4), occluded in rock salt. To date, the rock salt samples analyzed have been relatively small (400- to 1,000-gram) grab samples from Louisiana Gulf Coast domal salt mines. The results obtained are comparable to results in Polish domal salt mines, in terms of occluded gas volumes per mass of rock salt. The notable difference between the Louisiana and Polish occluded gas mixtures is in the relative proportions of the individual gas species. The two methods used by the Bureau are ballmill crushing and dissolution. Of the two, the dissolution method appears to be more versatile because it can be performed in situ. The relevance and applicability of data on the occluded gas contents of rock salt are dependent on sample size, sample collection method, geologic context of the sample, and the correlation with gas emissions that occur as a result of mining-induced fractures and pressure differentials.

Jan 1, 1982

By Fred Leighton

The Bureau of Mines monitored a rock-burst-prone pillar in a metallic ore vein, up to and through failure, to measure its reactions to increasing loads, as it was mined. Three parameters were monitored: the stress changes at chosen points within the pillar, the displacement characteristics of the drift above the pillar, and the micro-seismic activity in and around the pillar. In descending order of effectiveness, the microseismic technique, vibrating wire stress measurements, and displacement measurements reflected the pillar reactions, and all showed good correlation to one another. A major rock burst in the pillar, which destroyed about 100 feet of drift above the pillar, occurred at the end of this study. This burst was preceded by a large anomaly in the microseismic activity in the failure area.

Jan 1, 1982

By Steven M. Shope

The Bureau of Mines electromagnetic trapped miner location and communications system requires a thorough understanding of through-the-earth electromagnetic wave propagation. An earth model incorporating a magnetic dipole buried in a three-layered earth has been developed. The dipole source is located in the second subsurface layer. By application of proper limiting values, the three-layered model is reduced to two different two-layered models and eventually to the homogeneous half-space model. The solutions are in the form of infinite integrals. A numerical analysis was carried out and a computer program written to evaluate the surface magnetic fields. Numerical values for the magnet- ic field at the point above the source are presented in a variety of models.

Jan 1, 1982