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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 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. C. Dahlin

The Bureau of Mines conducted laboratory batch beneficiation tests on samples from four potential platinum resources in southeastern Alaska to concentrate platinum and other precious metals. Thin Investigation was done as part of the mission of the Bureau to insure an adequate supply of minerals to meet the Nation's needs. Petrographic studies and beneficiation methods including gravity concentration, froth flotation, and magnetic separation were used to determine mineral association and to attempt to concentrate the platinum values with a primary mineral value such as chromite, copper sulfide, or magnetite. A high-graded sample from the Salt Chuck copper sulfide deposit yielded the platinum-group metal concentrate; the maximum grade attained was 0.04 oz Pt and 1.5 oz Pd per ton of high-grade copper sulfide concentrate. The other samples yielded low-grade primary mineral concentrates with low platinum-group values, and/or the platinum-group metals did not concentrate with the primary mineral value.

Jan 1, 1981

By W. E. Anable

The Bureau of Mines researched methods for recovering copper from cyclone and electrostatic-precipitator dusts of primary copper smelters as part of its program to maximize minerals and metals recovery from primary and secondary domestic resources. Small-scale studies showed that use of 110 pct stoichiometric sulfur and 123 pct stoichiometric carbon, based on producing a 40-pct copper-iron matte, resulted in the recovery of 95 pct of the copper contained in the dust. Typical mattes contained less than 10 pct of the arsenic, 30 pct of the bismuth, and 45 pct of the antimony and tin contained in the dust. Matte was converted to blister copper by injecting up to 200 pct of the stoichiometric oxygen requirement over a period of 2 to 3 hours. Up to 76 pct of the copper contained in the dust was recovered as a crude blister copper containing about 2 pct arsenic, 0.5 pct antimony, and less than 0.1 pet bismuth and tin. A matte-white metal product resulted from carbothermically reducing dust with coal, lime, and silica. Up to 95 pct of the copper was recovered in the combined product.

Jan 1, 1981

By H. B. Salisbury

As a part of a research program designed to help minimize national requirements for new mineral commodities by maximizing recovery of metals from domestic secondary resources, the Bureau of Mines investigated the development of economic methods for recovering copper and associated metals from complex electronic scrap. Three types were selected for research: (1) multiple-pin plugs and connectors, (2) obsolete aircraft radio assemblies, and (3) the magnetic fraction of shredded electronic scrap furnished by the Bureau's Avondale Research Center. The plugs and connectors, after incineration to remove plastic components and melting, yielded a brittle ingot, as did the internal portion of the radio assemblies. The brittle ingots were ground to minus 35-mesh for processing, and the magnetic material was used in the as-received condition. A process using pretreated or raw scrap as a copper precipitant in various concentrations of acidulated copper sulfate solution was developed as a means of effecting an initial separation and upgrading in the form of high-grade cement copper containing all or most of the precious metals.

Jan 1, 1981

By L. L. Brown

As part of the Federal effort to help maintain an adequate supply of fertilizer materials, the Bureau of Mines conducted research to characterize complex low-grade Michigan phosphate materials and to devise methods for recovering fertilizer-grade phosphate concentrates. The rock is from middle Precambrian sedimentary formations in the Marquette Range located in the central part of the Upper Peninsula of Michigan. Occurrence of phosphate-bearing sediments in Precambrian rocks is rare. This deposit, containing 12 to 15 pct P205, is believed to be the richest Precambrian phosphate deposit in the United States. Petrographic examination showed that the conglomeritic rock contains crystalline apatite both in "black pebbles" and in quartz matrix. Attrition scrubbing and sizing tests showed that there is no tendency for phosphate to concentrate in any of the sized fractions. In beneficiation tests, which included grinding to minus 325 mesh followed by phosphate mineral flotation using a fatty acid-fuel oil collector, a phosphate concentrate was obtained that had a grade of 30 pct P205 and a P205 recovery of 72 pct. This concentrate should be suitable for fertilizer manufacture.

Jan 1, 1981

By John Durkin

This report discusses the configuration and system deployment for the postdisaster surface seismic system for detecting and locating trapped miners. It analyzes the results of 15 field tests to define a signal model, background noise levels, and subarray performance. A waveform modeling procedure is described and compared with observed waveforms. The resulting similarity indicates that the major factors affecting the signal amplitude, waveform, and spectral character are understood. A model is presented which gives the sig-nal amplitude as a function of source type, source depth, and horizontal off-set between source and receiver. Using this model a curve is presented which gives the range at which a signal will be detected for different signal and noise levels. Finally, and most important relative to the mission of the system, the ability of the system to detect signals on one or more subarrays is put into a probabilistic framework. For a strong source it is almost certain that a subarray directly over the source will detect the signal. After signal processing, it is highly likely that signals will be detected on sufficient subarrays to locate the trapped miner. Location errors have been found to be less than 100 ft in the majority of cases. Techniques have been used that can reduce the location errors to this level even when soil layer variation between subarrays is severe.

Jan 1, 1981

By G. A. Savanick

The Bureau of Mines has designed, fabricated, and field tested a water jet cutting device capable of perforating nonmetallic well casings for the purpose of completing or stimulating in situ uranium leaching wells. The device is lowered into the wellbore, where it issues a high-velocity water jet that penetrates either a polyvinyl chloride or fiberglass casing, cement, and from 1 to 4 feet into the surrounding uraniferous sandstone. The resulting perforations allow leaching solution to pass between the sandstone and the wellbore. This report describes the water jet perforator, tells how it is used, presents cost data, and discusses the results of laboratory and field tests. The tests were designed to (1) determine the optimum operating conditions for water jet perforation, (2) assess the effects of changes in these conditions, (3) evaluate the performance of the water jet perforator under actual conditions, and (4) compare this method with other methods of well completion. These tests showed that water jet perforation is superior to conventional well completion methods for selectively achieving communication between the well-bore and adjacent sand while maintaining sand control, for restoring permeability lost through wellbore damage, for stimulating poorly performing wells for completing wells with casings that have inside diameters as small as 2 inches, and for extending the effective well diameter.

Jan 1, 1981

By J. J. deBarbadillo

This Bureau of Mines report describes a process for recovering chromium and other metals from superalloy scrap. Laboratory-scale experiments were conducted to test a complex flowsheet utilizing a wide range of extractive metallurgical operations. The novel basis for the process is the fonnation of a sulfide matte in which chromium is concentrated in a discrete chromium sulfide phase. Mineral processing and hydrometallurgical procedures are used to separate chromium sulfide from the other matte constituents. The products of the process are a chromium-nickel alloy suitable for reuse in the superalloy industry, electrolytic nickel, electrolytic cobalt, and iron-molybdenum residue. Recovery of the principal elements contained in the scrap is chromium--93 percent, nickel--99 percent, cobalt--96 percent, and molybdenum--92 percent.

Jan 1, 1981

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

By Seth C. Schaefer

The Bureau of Mines has determined the standard Gibbs energies (AGf°) of CoS1.035 (cobalt sulfide) and Ni2.515S2 (nickel sulfide) with high-temperature galvanic cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, CoS1.035, CoO, S02(g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt, with the overall cell reaction C0S1.035(c) + 1.535 02(g, 0.0114 atm) = CoO(c) + 1.035 S02(g)¬ These results, combined with the best available data for ?Gf° of CoO and S02 from the literature, give the standard Gibbs energy of formation of CoS1.035 for the reaction Co(c) + 0 5175 S2(g) = CoS1.035(c) ?Gf° = -38.890 + 18.87 x 10-3T ± 0.185 kcal/mole (866.0 - 1,104.9 K), where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, N12.515S2, NiO, S02(g, 1 atm)//Zr02//02(g, 0.0122 atm), Pt, with the overall cell reaction Ni2.515S2(c) + 3.2575 02(g, 0.0122 atm) = 2.515 NiO(c) + 2 S02(g). Combination of these results with data for ?Gfo of NiO and S02 from the literature yields the standard Gibbs energy of formation of Ni2.515S2 for the reaction 2.515 Ni(c) + S2(g) = Ni2.S1SS2(c) ?Gf° -65.377 + 24.67 x 10-3T ± 0.541 kcal/mole (968.6 -1,053.7 K).

Jan 1, 1981

By C. Melvin Lepper

To provide the U.S. mining and energy industries with information in the selection of seismic detectors for high-resolution applications, the Bureau of Mines evaluated 35 velocity detectors (geophones) and 9 accelerometers. It was found that velocity detectors with natural frequencies from 10 to 100 Hz were effective for seismic studies in the 5-to 600-Hz spectrum and that accelerometers were most effective in the 100-to 1,000-Hz range. Although the accelerometers described in this report performed about equally with the better velocity detectors tested, the accelerometers showed higher output voltage levels at higher frequencies, which is an advantage. It is important that a seismic detector and its intended purpose be matched properly to achieve the intended results in high-resolution applications. There are many factors that could affect proper matching, thus careful selection of the best detector for a particular application must be exercised.

Jan 1, 1981

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolanic-cement concrete to develop a low-strength backfill. Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan (fly ash) and lime. Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressive-strength curves that can be used to estimate the best backfill mix for any mine.

Jan 1, 1981

By E. R. Cole

Bench-scale research at the Bureau of Mines has resulted in the successful development of a combination electrorefining-electrowinning method for recycling all the lead in scrap batteries. The method reduces energy consumption and eliminates toxic emissions, in contrast to present pyrometallurgical smelting, and the lead produced is pure enough for use in maintenance-free batteries. Anodes cast from molten lead scrap were electrorefined in 1-and 2-liter plastic cells using an electrolyte composition of 70 g/l Pb and 90 g/l free H2SiF6 (fluosilicic acid). Both reagent-grade and waste H2SiF6 were used. Cathode starting sheets were made from refined lead. Aloes, and later bone gelatin, and calcium lignin sulfonate addition agents were employed. The sludge remaining after separation of the lead metal was treated in a two-step leaching operation to solubilize the lead for recovery by electrowinning. Conditions for electrowinning were essentially the same as for electro-refining, except that insoluble Pb02-Ti (lead dioxide-coated titanium) anodes were used. The best results for both electrorefining and electrowinning were obtained with a current density of 170 amp/m2 and a cell temperature of 25° to 35° C. Cathode purity ranged from about 99.9 to 99.99+ pct Pb. Maximum energy consumption after 3 days, for electrorefining and electrowinning, was 90 and 700 kwhr per metric ton of refined lead, respectively.

Jan 1, 1981

By William D. Riley

In order to evaluate the corrosion resistance of zirconium in mineral extraction processes, such as a clay-hydrochloric acid leaching process for extracting alumina, the Bureau of Mines conducted corrosion studies in HCl-AlC13-FeC13 environments. A series of weight loss and electrochemical tests were conducted at 25° and 65° C in aluminum chloride (AlC13) plus hydrochloric acid (HCl) solutions containing 0 to 1,000 ppm ferric ion. It was determined that zirconium, which normally exists in a passive state in chloride-containing solutions, undergoes pitting attack in solutions containing more than 100 ppm of ferric ion. It is also shown that an oxide film prepared in air at high temperature offers protection in acid solutions containing levels of ferric ion from 300 to 1,000 ppm.

Jan 1, 1981

By G. R. Palmer

Preliminary studies by the Bureau of Mines were conducted to determine the feasibility of a multiple-compartment, ion-exchange (MCIX) column simulator for examining the effect of multiple-orifice plates in the column. A rectangular, five-orifice, three-compartment, MCIX simulator with a cross-sectional plate area of 0.66 ft2 was used for the investigation. Orifices with open areas of 1, 3, and 5 percent were used with various operating conditions. The study was separated into three separate sections: (1) solution flow effect, (2) fluidization effect, and (3) resin transfer effect. The solution flow and fluidization studies showed that for solution flow rates of about 3 gpm/ft2, a I-percent open area plate functioned best, while at solution flow rates of 9 and 15 gpm/ft2, the best open areas were 3 and 5 percent, respectively.

Jan 1, 1981

By J. M. Kuchta

The Bureau of Mines investigated four simulated coal gob fires to obtain a more reliable data base for defining the state of a sealed mine fire and to evaluate the performance of various fire detectors. The fires were conducted in a multiple-entry section of the Bruceton Experimental Mine by heating 4,000 to 21,000 pounds of rubblized bituminous coal to ignition and monitoring the temperature, gas emissions, and smoke under ventilated and sealed combustion conditions. Product gas concentrations depended upon the coal bed size, coal temperature, heating rate, and oxygen concentration or ventilating condition but varied little after the fires were sealed. Expressions are given that define the temporal variation of CO and O2 after sealing when the coal temperature decreased rapidly. The CO/C02 ratio is a more sensitive fire indicator than the CO/?02 ratio, although the latter is universally used for detecting the incipient state of a coal fire. In comparison, the Jones-Trlckett ratio [ CO2 + ¾ CO ? ¼ H2 ?O2] is less reliable for this purpose. The best detector for determining the state of a mine fire after it has been sealed was a prototype submicrometer smoke particulate sensor. Limitations of the various detector systems are also discussed.

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 Robert W. Waytulonis

The Federal Bureau of Mines contacted 29 organizations--mine maintenance departments and equipment manufacturers--concerning service experience and construction of diesel exhaust-gas water scrubbers. Scrubbers are used primarily on mobile diesel-powered mining equipment subject to 30 CFR 36. Because the scrubbers cool exhaust gas and act as flame arresters, their failure would compromise safety in underground mines. Scrubber maintenance problems and frequency and modes of failure were identified, and construction materials and techniques were evaluated. Three failed scrubbers were randomly selected from two cooperating mines, and their modes of failure were determined. In conjunction with failure analyses, mine water and scrubber water solution samples were chemically analyzed to characterize corrosive properties. Sludge and mineral deposits and different types of corrosion and metal fatigue were identified as problems leading to scrubber failure. The corrosion process is explained; maintenance practices, construction materials, and manufacturing methods that could be used to reduce premature failures and allow longer effective scrubber life are identified; and basic changes in scrubber design are suggested. If type 304 stainless steel is used throughout the scrubber and regular maintenance is performed, long, dependable service can be expected. Other materials such as 304L, 316, or other more exotic steel alloys may be necessary under certain conditions.

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