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By S. E. Khalafalla

The Bureau of Mines has used colloidal solutions of magnetite in a magnetic field to segregate nonmagnetic materials such as nonferrous scrap metals and to concentrate precious minerals. Conventional magnetic separation relies on the inherent magnetic susceptibility of the material to be separated and may be designated as magnetic separation of the first kind the medium of separation rather than the separated particles are made magnetizable, a new system of gravity separation results. In this new magnetic separation of the second kind, a magnetic fluid rather than air or water acts as the separation medium. The same force that attracts magnetic objects in separations of the first kind also attracts the entire separation medium in separations of the second kind, thereby creating a reactionary force of equal magnitude in the opposite direction. This force, sometimes called the levitation force, can be made to segregate nonmagnetic particles in a flowing stream according to their specific gravity. The technique has been applied to segregate nonferrous metals from automobile and appliance shredders and mixed scraps. The system has also been used to upgrade diamondiferous jig concentrates from certain river gravels in order to facilitate the sorting and recovery of their diamond content.

Jan 1, 1981

By A. E. Raddatz

In an attempt to develop technology to use domestic resources in place of imported bauxita, the Bureau of Mines investigated sulfurous acid leaching to extract alumina from kaolin. The process consists of leaching the calcined kaolin with a 30 wt-pct S02 solution at 60° C and 160 psig for 17 hours, fil¬tering the leach slurry, precipitating monobasic aluminum sulfite from the filtrate at 110° C and 60 psig, a& decomposing the sulfite in the spent liq¬uor at 150° C and 55 psig to produce crude alumina. Purification of the crude alumina was accomplished using a modified Bayer process. Results from closed-circuit tests employing the sulfurous acid process showed that overall extraction of alumina from kaolin was 67 pct. Production of 1 ton of alumina would require 3.6 tons of calcined kaolin, 0.7 ton of sul¬fur dioxide, and 8.4 tons of water. After purification by a modified Bayer process, the alumina product contained the following; impurities, expressed in weight-percent: Fa203, 0.009; S, 3.6; Si02, 0.07; Ti02, 0.002; K20, 0.017; and P205, 0.03.

Jan 1, 1981

By Philip C. Good

The Bureau of Mines investigated the feasibility of utilizing low-grade phosphatic shale as a feed for phosphoric acid production. Present practice in the phosphate mining operations of southeastern Idaho is to remove and either stockpile or waste low-grade phosphatic shales as the high-grade phosphate beds are selectively mined. Acid digestion studies were performed on uncalcined shale and on shale calcined to remove free carbon to determine phosphoric acid quality, yield, and amenability to filtration. The untreated shale, containing 21.4 pct P205, was digested with sulfuric acid in a single-tank reactor to yield phosporic acid and gypsum residue. Although 96 pct P205 recovery was attained in digesting uncalcined shale, only the calcined product gave satisfactory filtration rates. Calcined shale yielded phosphoric acid recovery of about 93 pct of the contained P205. It was higher in impurities than commercially prepared acid derived from high-grade western phosphate rock. An acid filtration rate of 745 lb P205/ft2/day was attained. This value is lower than the rate of 900 lb P205/ft that is generally considered to be acceptable in industrial production of phosphoric acid from high-grade phosphate rock.

Jan 1, 1981

By D. A. Stanley

The Bureau of Mines conducted laboratory-scale experiments to determine whether or not surface waters with a high organic content could be purified sufficiently to be used to replace the natural high-quality deep well water currently being used in the silica flotation step of phosphate rock beneficiation. Waters abundant in organic matter were collected from two central Florida streams, flocculated with a cationic polyethylenimine polymer, and processed in a sand filter. This treatment removed most of the organic materials from the water. Untreated surface water, treated surface water, and distilled water were used to compare the flotation response of the acid insolubles in an amine flotation circuit. Surface water treated with PEI-1000 was shown to be as effective as distilled water for the acid-insoluble-flotation step. Flocculation and filtration can therefore produce water suitable for amine flotation of quartz, which would permit substitution of surface water for deep well water.

Jan 1, 1981

By N. I. Jayaraman

High-pressure shrouded sprays were first tested on a bench to determine air-moving capability and dust collection efficiency. The bench-scale tests indicated that at 500 psi and above, the dust collection efficiency, when sampled downstream of a water eliminator, was about 99 pet for two types of nozzles. However, for the same water flow, the induced airflow was about three times greater in one type than in another. Since the only difference in the nozzles was the spray angle, this factor was important in air movement through a shrouded spray. Full-scale model mine tests were then conducted to determine the reduction in dust concentration behind the line curtain and at the operator position produced by high-pressure sprays in a shroud. The shroud was mounted on top of the boom of a model continuous miner, and high-pressure (greater than 500 psi) sprays were installed inside the shroud. The inlet of dusty air to the shroud was open toward the face and the outlet toward the exhaust line curtain. The high-pressure sprays were compared with conventional sprays mounted at the head of the continuous miner and directing water toward the face. The difference at the operator position (opposite side of brattice) was significant in that, under certain conditions, with conventional sprays an increase in respirable dust concentration of 471 pet was noticed compared with dry operation due to rollback from face. High-pressure shrouded sprays, on the other hand, decreased the dust concentrations at the operator position (opposite side of brattice) by 28.2 pct.

Jan 1, 1981

By D. R. Flinn

A newly developed chemical conditioning technique, which greatly simplifies the preparation of plating baths for the electrodeposition of titanium diboride (TiB2) coatings, is described in this report. The new plating technique was used to prepare samples of titanium diboride (TiB2) coatings on three types of substrate materials. These samples were then evaluated in both low- and high-speed wear-test programs to determine the wear resistance, microhardness, and adhesion of the coatings. In general, it was found that the wear resistance of the coatings is independent of substrate. Scanning electron micrographs have shown that the coating wear surfaces are very smooth, suggesting slow and continuous removal of the coating during the wear test (that is, adhesive wear). Adhesion between the coating and all substrates was excellent. Microhardness results show that the TiB2 coating is harder than alumina, with a hardness value exceeding 5,000 kg/mm2 measured in one test. The results of the wear tests show that TiB2 coatings have relatively poor wear resistance compared with alumina in low-speed unlubricated sliding environments, but exhibit wear properties comparable with alumina in high-speed unlubricated sliding environments.

Jan 1, 1981

By I. Liebman

The Bureau of Mines conducted experiments on coal dust explosion suppression. The investigation took place on a beltway in the double-entry of the Bureau's Experimental Mine. Using conditions that simulate those in a working mine, the investigation showed that a coal dust explosion can be readily initiated in a conveyor belt entry. Also, the explosion can spread into adjacent entries through opened crosscuts (stopping destroyed by explosion) to propagate for long distances even though the adjacent entries are rock dusted in compliance with regulations. Passive water barriers (water-filled tubs) were found to be effective in suppressing explosions on a beltway; however, barrier efficiency was reduced by opened crosscuts. The study indicated that the beltway barrier should be the distributed type consisting of continuous rows of water-filled tubs covering long distances along the entry. A plan is outlined for the installation of a water barrier system in a working coal mine for the protection of a beltway.

Jan 1, 1981

By S. R. Crane

One Bureau of Mines goal is to minimize the undesirable environmental impacts associated with industrial plants emitting waste gases containing S02. To help meet this goal, a regenerable flue gas desulfurization process was developed. This process, known as the citrate process, uses a buffered weak acid solution to absorb S02 from the waste gas. The absorbed S02 is reacted with H2S to precipitate elemental sulfur and regenerate the solution for recycle. The H2S feedstock for the process, if not otherwise available, may be produced by reacting two-thirds of the recovered elemental sulfur with natural gas and steam. Laboratory investigations and pilot plant operations were conducted by the Bureau to determine if H2S from the natural gas, sulfur, and steam reaction was suitable for the citrate process. The laboratory investigations, in which an H2S generator was integrated with other citrate process operations, provided a basis for design and operation of the pilot plant. The objective of the pilot plant was primarily to provide H2S for the citrate pro-cess pilot plant at the Bunker Hill Co. lead smelter in Kellogg, Idaho. The design capacity of the pilot plant was 0.4 to 1.25 tons of H2S per day. The operation demonstrated that (1) a 77-to 79-dry-volume-percent H2S product could be produced from pilot-plant product sulfur, natural gas, and steam; (2) the product R2S regenerated the SO2-loaded citrate solution; and (3) under certain conditions over 95 percent of the natural gas could be converted to H2S.

Jan 1, 1981

By W. N. Marchant

The Bureau of Mines performed chemical research to elaborate details of sulfur chemistry pertaining to the citrate flue gas desulfurization process in which sulfur dioxide (SO2), absorbed (as bisulfite ion) in a buffered sodium citrate solution, is reduced by hydrogen sulfide (H2S) according to the overall reaction 2H2S + HSO3 + H+ ? 3S + 3H20. The rate-limiting step in the process was shown to be the reduction by H2S of thiosulfate (S2031-) that is formed as an intermediate. Pseudo first-order kinetic measurements were made at room temperature to retard the reaction sufficiently that adequate analysis was possible. These measurements showed the rates of the following net processes to be -d [S02]/dt (pH 4.5) = (0.409±0.050)min-1 [S02]; d [S2032-]/dt (pH 4.5) = (0.199±0.017)min-1 [S02]; -d [S2032-]/dt (pH 4.0) = (0.0437±0.0265)min-1 [S2032-]~1; -dH2S/dt (pH 3.9) = (21.6±3.0) mmoles/min-atm [H2S]g1.4, where [H2S]g is the partial pressure of H2S in the gas phase, in atmospheres, and the rate describes the consumption of H2S, in millimoles per minute; d[S]/dt (pH 4.0) = (38.0±3.4)min-1 [H2S]1, where [H2S] is the concentration of H2S in solution. Hydrogen ion consumption during the slow phase of regeneration was shown to occur at (2.1±0.5) times he rate of thiosulfate consumption, which is interpreted as evidence for the following as the rate-limiting reaction: 2H2S + S2032- + 2H+ ? 4S + 3H20 A scheme consisting of five sequential general reactions is proposed to account for sulfur formation.

Jan 1, 1981

By E. D. Calvert

The Bureau of Mines, in its effort to promote greater utilization of domestically abundant materials, conducted reasearch on an alternate mold material that has commercial potential for titanium investment casting. Using variations of the conventional lost wax molding process, investment shell molds were formed entirely of fused, calcia-stabilized Zr02 and a Zr02-forming binder. Optimization of binder/slurry properties', stucco grain size and dis¬tribution, and curing practices resulted in a structurally sound investment shell that was distortion free and thermally stable. Small titanium castings, weighing up to 10 pounds, were prepared in unheated molds by both static and centrifugal casting techniques. Microstruc¬tural examination of the castings revealed that mold fill and surface quality were enhanced by centrifugal casting, although good results also were obtained from the statically poured molds. Microstructural and electron microprobe examinations showed that excessive, brittle case formation could be avoided by curing the dried shell molds in air for at least 2 hours at 1,400° C. Increasing curing temperature and time above these levels yielded added bene¬fits. Molds fired in vacuum at 1,500° C for 4 hours yielded castings essen¬tially free of case formation. The tensile properties of as-cast test specimens (no surface conditioning performed) id the chemical composition of representative metal samples showed that castings produced were comparable to Grades C-1 and C-2 unalloyed titanium This indicated that no sifnificant degradation of metal properties resulted from mold/metal interaction.

Jan 1, 1981

By Kenneth L. Cashdollar

This report describes three types of optical dust probes that have been designed, built, and tested by the Bureau of Mines. Each of the probes measures dust cloud concentrations by the attentuation of light. The first is a single-path-length probe, the second is a double-path-length probe, and the third is a single-path-length probe that employs jets of air to keep the windows of the light source and detector free from dust coating. The theory of operation and the calibration procedures for each of the probes are described. The results of the Bureaus laboratory, mine, and field tests of the probes are also reported.

Jan 1, 1981

By Arne Landsberg

The Bureau of Mines has undertaken research to elucidate the chemistry involved in the efficient recovery and control of minor elements in base metal smelting operations. These elements should be effectively recovered not only because they have commercial value, but also because of their potential hazard to workers' health and the environment, if they are not controlled during processing. Cadmium, a minor metal in zinc ores, is the subject of this report. The roasting step of the complex zinc-smelting process was chosen for investigation because of the high potential for removing cadmium by volatilization during this primary stage. Commercial roaster feed materials were used to determine the sequence of reactions and the effect of these reactions on the volatilization of cadmium. Electron microprobe examination of both the commercial roaster product and oxidized sulfide solid solutions prepared in the laboratory showed that oxidized iron was of prime importance in preventing cadmium volatilization. The mechanism by which iron prevents cadmium volatilization is proposed, and a preheating technique is recommended for more effectively recovering cadmium prior to roasting.

Jan 1, 1981

By R. A. Bloomfield

This report summarizes Bureau of Mines contract research on the disposal of retorted oil shale. A data base has been developed describing the physical-chemical properties, geotechnical engineering properties, and natural cementation characteristics of spent shale. Results of field compaction tests and seepage pond tests are presented, along with results of a partially saturated finite element seepage model used to predict infiltration and seepage rates. Preliminary engineering analyses are presented for underground disposal systems, which include material transport methods, and for a surface disposal system, which includes stability analyses.

Jan 1, 1981

By W. C. McBee

A family of modified-sulfur cements has been developed by the Bureau of Mines for the preparation of construction materials with improved properties. Various types of sulfur cements were prepared by reacting sulfur with mixtures of dicyclopentadiene (DCPD) and oligomers of cyclopentadiene (CPD). Durable cements were prepared with structural characteristics ranging from rigid to flexible. These cements were used to prepare corrosion-resistant materials for use in a wide variety of industrial applications where resistance to acidic and salt conditions is needed. These materials were prepared as rigid concretes, flexible pavings, spray coatings, and grouts. Production of modified-sulfur cements in a commercial-size plant was demonstrated.

Jan 1, 1981

By B. W. Jong

As part of the Bureau of Mines program to develop substitutes for critical and strategic materials for metallurgical applications, the Tuscaloosa Research Center has evaluated the effect of additives and starting materials on the sintering and strength properties of sialon (silicon-aluminum-oxynitride) compositions fabricated by conventional pressing and sintering techniques. Sintering and MOR (modulus of rupture) data were developed for sialon compositions produced from three components, Si3N4, A1203, and AIN. When doped with Y203 to aid in sintering, the highest MOR values were obtained with compositions containing between 20 and 30 mole-pet (A1203 + AIN). The effect of the crystalline phase of the Si3N4 and Al203 used in the three-component system on MOR also was investigated. Alpha-Si3N4 and ?-A1203 were found to be the best starting materials. A sialon composed of 67.4 mole-pct a-Si3N4 plus 32.6 mole-pct (?-AI203 + AIN), doped with 5 wt pct Y203, had MOR values at 25°, 1,200°, and 1,400° C of 40,300, 40,300, and 31,100 psi, respectively. Samples of this composition doped with Gd203, MgO, Zr02, and ZrSi04 also were evaluated. The ZrSi04-doped sialon had higher MOR values than Gd203-, MgO-, and Zr02-doped materials but lower MOR values than the Y203-doped sialon. The MOR values of ZrSi04-doped sialons were 25,000 and 25,900 psi, respectively, at 25° and 1,400° C.

Jan 1, 1981

By B. W. Madsen

To help maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines developed a mathematical model that describes acidic ferric sulfate leaching of copper from sulfide ores. The leaching model can aid in maximizing minerals and metals recovery from primary sources by giving operators and management a better understanding of the copper leaching process. This will aid in improving dump leaching operations. The model is based on a steady-state approximation of the continuity equation for diffusion of ferric ions in the rock pores and the intrinsic leaching kinetics of the various sulfide mineral particles. Ore characteristics included in the model were ore particle-size distribution, particle shape, grade, mineral content, mineral particle size, porosity, and tortuosity. The continuity equation was used with ferric ion concentration gradients and a fixed value for the diffusion coefficient. Except for effective diffusivity, each of these factors was either measured experimentally or estimated from theoretical considerations. The effective diffusivities were determined by fitting calculated leaching curves with experimental leaching data. Vertical variations in leach solution composition and temperature within a dump are not considered in this model. The model accurately predicted copper extractions for several large-scale tests during nearly 500 days of leaching.

Jan 1, 1981

By Harold L. Rhodes

The Bureau of Mines has developed a quantitative method to determine water vapor in helium in the range of 0.1 to 15 ppm by volume. This method uses the quantitative chemical reaction of H20 with CaH2, which produces 1 mole of hydrogen for each mole of H20 in the sample. A gas chromatograph is then used to determine the concentration of hydrogen in the product. The precision of the H20 analysis is ±0.05 ppm at a concentration of 1 ppm. This method is used to calibrate a commercial platinum-phosphorus pentoxide (Pt-P205) electrolytic water vapor analyzer that has an improved inlet system and digital voltmeter readout.

Jan 1, 1981

By R. E. Peterson

A reduction roasting/magnetic separation/flotation process for beneficiating oxidized taconite from the western Mesabi iron range in Minnesota was evaluated in a Bureau of Mines research program to insure an adequate supply of raw materials for future ironmaking and steelmaking needs. The research was performed on a sample containing 35.4 pct iron and representing a deposit of approximately 2 billion tons of raw materials. An average of 1,419 lb of oxidized taconite and 37 lb of lignite reluctant per hour were fed to a 35 -foot rotary kiln in which the iron oxides were converted to artificial magnetite. The kiln was heated with pulverized lignite and natural gas. Most of the dust collected from the kiln exhaust gas was pelletized and recycled to the kiln. Magnetic separation and cationic flotation of the roasted material in a 900-lb/hr pilot plant produced a concentrate analyzing 67.9 pct iron and 4.9 pct silica and containing 69.2 pct of the iron in the kiln feed.

Jan 1, 1981

By D. E. Shanks

As part of its program to lessen dependence on foreign bauxite as the Nation's primary source of cell-grade alumina, the Bureau of Mines is investigating sulfuric acid (H2S04) leaching procedures for the recovery of alumina from domestic aluminous materials. The successful application of a H2S04 leaching process depends on the recovery of the aluminum values in an easily washed and filtered form, containing a minimum of water to be driven off in the subsequent calcination step. This goal was met by the high-temperature hydrolysis of simulated aluminum sulfate [A12(S04)3] leach liquor. Crystalline, insoluble aluminum hydroxy sulfate [A1(OH)S04], which had a water-to-alumina mole ratio of 1:1, was produced. Eighty-six percent of a solution containing 127 g of A12(S04)3 per liter and 76 pct of a solution containing 336 g of A12(S04)3 per liter were hydrolyzed to insoluble aluminum hydroxy sulfate by autoclaving for 1 hr at 320° C and rapidly quenching to room temperature. Higher operating temperatures were precluded by corrosion of the autoclave. The yield of aluminum in the hydrolysis product increased with increasing hydrolysis temperature and decreasing A12(S04)3 concentration.

Jan 1, 1981

By J. F. Papp

The microstructures of a CF2Br2-inhibited methane flame and its uninhibited analog have been determined using molecular beam-mass spectrometry. The slightly lean flames were stabilized on a cooled porous plug burner at reduced pressure. Composition profiles of stable, intermediate, and radical species and temperature profiles were obtained. Comparisons of the uninhibited and inhibited flame profiles revealed the following inhibition effects; a shift of the primary reaction zone to higher temperatures, a higher maximum flame temperature, an increase in the CH3 concentration, and a reduction in the H2CO, H, 0, and OH concentrations. Kinetic analyses of the data yielded rate coefficients at flame temperatures for the reactions H + CH4 ? CH3 + H2, H + O2 ? OH + O, CO + OH ? CO2 + H, and CH3 + O ? H2CO + H. CF2Br2 is judged to decay by thermal decomposition and abstraction reactions.

Jan 1, 1981