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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

By Howard D. Jacobs

A bulk sample of oxidized taconite taken from the western Mesabi Range was evaluated by the Bureau of Mines using the Bureau-developed selective flocculation-desliming-cationic (or anionic) flotation process. The raw ore sample containing 32.3 pct Fe was treated by both cationic and anionic flotation. Using the cationic system the concentrates averaged. 37.2 wt-pct of the feed and contained 62.8 pct Fe and 4.7 pet Si02 with an iron recovery of 72.3 pet. With the anionic system, concentrates averaged 37.7 wt-pet of the feed and contained 63.0 pct Fe and 5.3 pct 8i02 with an iron recovery of 73.5 pct. A comparison of reagent costs showed that the cationic process cost 144.1 cents per long ton of crude ore and the anionic process 178.7 cents per long ton of crude ore. Reclaimed water comprised 86 pct of the total water requirement for anionic flotation and 88 pct for cationic flotation. The ore used in this study was one of three samples representing about 3.25 billion tons of oxidized taconite containing from 32 to 36 pct feed iron. Previous study had indicated that selective flocculation-desliming-cationic flotation would produce concentrates from the other two samples of 61.7 pct Fe and 5.1 pct Si02 at 67-pct Fe recovery, and 63.5 pct Fe and 4.3 pet Si02 at 8S-pct Fe recovery. By developing a successful treatment for these ores, the Bureau has insured the availability of technology for processing an amount of raw iron ore which, by itself, would supply U.S iron needs for 50 to 75 years at expected consumption rates.

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 J. F. McIlwain

As part of its goal to minimize the requirements for critical materials, the Federal Bureau of Mines has investigated the consolidation of an iron-base superalloy (20 pct Cr, 5 pct each Ni and Mn, 1 pct each C, W, Mo, and Cb, and the balance Fe) and its modifications by powder metallurgy (P/M) techniques. Vacuum-atomized, prealloyed powder was used. Consolidation was by sintering of cold-pressed alloy powder, or by forging plus rolling or extrusion of canned powder. Several commercial lubricants were evaluated in the pressing operation. At 50-tsi compacting pressure with up to 3 wt-pct lubricant, green strengths did not exceed 1,000 psi. Powder sintered just below the solidus temperature attained a tensile strength of 69,000 psi and 4 pct elongation. Liquid-phase sintering produced higher densities, lower tensile strengths, and nil ductility. Canned powder was forged and rolled at 1,200° C, yielding a 100-hr rup¬ture strength of 9,800 psi at 815° C and a room-temperature tensile strength of >130,000 psi at 6 pct elongation. Heat treatment of modified P/M iron-base alloy containing 0.63 pct C resulted in a 100-hr rupture strength of 17,000 psi. Oxidation resistance at 805° to 815° C of the forged and rolled P/M iron-base alloy was similar to that of the cast iron-base alloy and supe¬rior to conventional stainless steels.

Jan 1, 1981

By E. G. Davis

A research program to evaluate the use of ceramic die inserts for ferrous diecasting was initiated by the Bureau of Mines at its Tuscaloosa Research Center. Data were compiled from the literature to characterize selected ceramic materials with respect to thermal properties, thermal-shock resistance factors, chemical reactions with molten metals, and processes required to form die components. With this information and a computer model developed for predicting temperature and stress patterns induced in ceramic materials during simulated ferrous diecasting operations, 27 candidate materials were evaluated. After evaluation, only 15 were considered for testing in an apparatus constructed to immerse the ceramic specimens in molten cast iron. Of these, 13 were tested in a modified testing unit in which cast iron was poured onto the specimens. These tests resulted in the selection of three materials for further testing: boron carbonitride (50 pct B4C:5O pct BN), boron nitride-grade M (BN-M, 40 pct BN, 60 pct Si02), and pyrolytic boron nitride (PBN). Tests in a gravity-flow die unit showed that PBN was thermal-shock resistant and could be used in diecasting of ferrous metals.

Jan 1, 1981

By H. W. Kilau

The Bureau of Mines evaluated synthetic fluorspars as substitutes for natural fluorspar in basic oxygen steelmaking using a high-temperature rotational viscometer and a quarter-ton basic oxygen furnace (BOF). Consider-able variation in stability and BOF slag fluidizing properties were found when using the initial synthetic products, but improved synthesis methods produced synthetic fluorspars that were generally comparable to natural fluorspar in laboratory testing. Trials in the furnace showed the synthetic products to be operationally the equivalent of natural fluorspar. Higher sulfur and phosphorus contents in some of the synthetic materials did not adversely affect the steel chemistry. Analyses of wet scrubber samples showed evidence that the pelletized synthetic fluorspars experienced greater physical and chemical disintegration than did natural fluorspar. It was also found that operation of a BOF without fluorspar is possible when making low-carbon steels because iron oxide is intrinsically generated as the slag fluidizer.

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 B. S. Covino

The Bureau of Mines has conducted a laboratory and field corrosion test¬ing program to determine materials of construction for the leaching and gas-sparging crystallization environments of the clay-HC1 process in order to more fully utilize the alumina from domestically available kaolinitic clays. Laboratory tests were used to determine the corrosion rates of 22 metals and alloys by weight-loss measurements in these two environments of the process. The results of this laboratory study were used both to suggest metals and alloys for field testing and to determine the effect of the individual solution components on the corrosion behavior of the metals and alloys. Results from the field tests were used to recommend Ta, Ta-2.5W, and Ta-10W for con¬struction of the agitators for the leaching process. The metals and alloys recommended for construction of the gas-sparging crystallizer heat exchangers were Ta, Ta-2.5W, Ta-10W, Nb, Nb-1Zr, Nb-3Zr, Nb-28Ta-10W-1Zr, Nb-10Hf-1Ti, and Zr for the first stage and Ta, Ta-2.5W, Ta-10W, Nb-28Ta-10W-1Zr, Nb, Nb-10Hf-1Ti, and Zr for the second stage.

Jan 1, 1981

By R. P. Beyer

As part of its thermodynamic investigations of mineral compounds, the Bureau of Mines has written an algorithm based on Newton's method for solving for the characteristic Debye temperature of a compound, from heat capacity and temperature data. A listing of a FORTRAN IV program based on this algorithm, for calculating Debye temperatures given heat capacities or for calculating heat capacities given Debye temperatures, is available from the author upon request.

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 Charles A. Seitz

This Bureau of Mines report describes an automatic and continuous transducer-drift compensator. The compensator formed a part of the instrumentation used to indicate the saturation by hydrogen of a cryogenic, adsorption column. It has a variable delayed-response characteristic and will respond only to signals having rise times faster than component drift times. Zero drift due to varying ambient conditions and component aging is nullified. Equations relating the output as a function of the input signal are given.

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