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By F. R. Cattoir

This Bureau of Mines study investigated molten salt electrorefining for beneficiating low-grade, high-carbon ferrochromium products which can be readily produced from domestic chromite concentrates. A second objective was to refine commercial ferrochromium into low-iron chromium products. Electrorefining of both types of ferrochromium in molten CaC12-NaCl-CrC12, CaCl2-MgC12-CrCl2, or KC1-LiCl-CrCl2 electrolytes produced chromium-iron products with virtual elimination of other impurity elements and some lowering of the iron content, Over 90 percent of the chromium present in the feed materials was recovered. The electrodeposited products were upgraded further by magnetic separation techniques into chromium containing less than 5 percent iron. The technical feasibility of preparing a premium chromium product from a low-grade, high-carbon ferrochromium made from domestic chromite was demonstrated. Chromium virtually free of carbon, oxygen, and silicon from high-carbon ferrochromiums was produced. In addition, the amenability of three commercial grades of ferrochromium to electrorefining and magnetic separation for preparing chromium metal containing less than 5 percent iron was determined.

Jan 1, 1969

By D. H. Desy

The Bureau of Mines studied the properties of copper that had been oxide dispersion-strengthened with 2 vol pct of either yttria or alumina. Compounds of copper and aluminum or yttrium, coprecipitated from aqueous solution, were converted to oxides; the copper was reduced, compacted, sintered, and extruded. For the resulting copper-dispersoid composites, room temperature tensile properties after annealing in hydrogen, elevated temperature tensile and stress-rupture properties, and electrical conductivity were determined. Compared with oxygen-free copper, copper-2 vol pct alumina or yttria had improved strength after annealing between 400° and 1,000° C, and improved elevated temperature strength, with little loss in electrical conductivity.

Jan 1, 1969

By Thys B. Johnson

Operations Research techniques for determining optimal shipping schedules and production and product allocation are discussed. A hypothetical mining operation model is formulated by the Bureau of Mines, and optimal production and product allocation are determined. The technique of sensitivity analysis is discussed and is used to illustrate the effect of the variability in a mining operation on the optimal production and product market plan.

Jan 1, 1969

By G. W. Weems

The Bureau of Mines used the Burnett method and apparatus to determine the compressibility factors for helium and carbon dioxide mixtures at 0°, 10°, 20°, 23°, and 35° C and to pressures of 900 psia. Tables of compressibility factors and approximations of the virial coefficients are presented for seven binary mixtures as well as for helium and carbon dioxide. The results compare favorably with existing data.

Jan 1, 1969

By M. J. Kovalik

Lower Sunnyside seam coal from Utah was blended with various proportions of char and high-temperature coke to improve the quality of the coke obtained from carbonizing this coal. The Hanson 5-pound carbonizer was used as a "screening test" for the larger scale Bureau of Mines-American Gas Association (BM-AGA) tests, which were correlated with industrial production. Eighteen carbonization tests were made in the BM-AGA 13-inch retort, with a coal charge of about 90 pounds; the cokes were evaluated by the standard ASTM tumbler test. Carbonization of blends containing char and coke breeze yielded less fissured and blockier cokes of significantly higher ASTM I-inch tumbler indices as compared with the value for the straight Sunnyside coal. It was found that the simultaneous addition of char and coke breeze yielded stronger cokes than that obtained by the addition of either one of these additives. Addition of a small proportion of Pocahontas No. 3 or Sewell coal to an optimum blend improved the resulting coke strength further.

Jan 1, 1969

By D. E. Wolfson

This report presents 900° C BM-AGA carbonization and related data for coals from the principal beds of Nicholas, Randolph, and Webster Counties, W. Va. Thirty-three samples from nine coal beds in three counties were car-bonized at 900° C in the l8-inch-diameter BM-AGA retort, data from which have been correlated with industrial production. Host of the samples were chemically suitable for metallurgical use, and their coking properties were satisfactory. Except for four of the Lower Kit-tanning samples, the ranges of constituents in the coal seams were 1.8 to 9.0 percent ash and 0.4 to 1.1 percent sulfur, values within the range of accept-ability for metallurgical coals. Coke strength indexes were normal for Appalachian coals of similar rank, and the tumbler stability indexes of the coke ranged from 35 to 57.

Jan 1, 1969

By Manuel Gomez

The Bureau of Mines used data from 31 core samples to develop prediction equations for evaluating chemical and carbonization properties of six seam units in a lignite deposit approximately 2 miles wide and 8 miles long in the Wilcox Formation of central Texas. Statistical response surfaces, based on core analyses, were computed for 14 parameters indicative of lignite quality. These computed surfaces, and their mathematical equations, can be used to predict values of the selected properties of the lignite seams at any desired surface coordinate position between core hole locations. The wide range of application shown by this study indicates that the methods of statistical regression analysis may be useful to evaluate large deposits of lignite or higher rank coal.

Jan 1, 1969

By R. L. Rough

The Bureau of Mines analyzed rotary-coring-operations data to compare mud and air as coring mediums, and to compare core recoveries, penetration rates, and cost data for the respective mediums as part of an investigation of the susceptibility to secondary-recovery techniques of petroleum reservoirs in Ohio, Pennsylvania, and West Virginia. This report describes the rotary-diamond coring equipment and operations employed while coring 20 wells--10 cored using mud, and 10 cored using air. Data relevant to the draw works, rotary-table power, drill pipe, drill collars, core barrel, core head, mud pumps, or air compressors are tabulated. Average bit weight and rotary speed, core recovery, and penetration rates are listed for each formation cored. In general, core recoveries were better from the mud-cored wells, whereas penetration rates were faster for the air-cored wells. Coring costs were about the same for single-formation wells cored with either mud or air; however, costs increased considerably when multiple-formation wells were cored with air.

Jan 1, 1969

By C. R. McCann

The Bureau of Mines conducted an experimental study of conditions needed to produce flames of pulverized coal when the heat needed for ignition is sup-plied only from the flame and hot furnace refractory. An electrically heated furnace which burned about 1 pound of coal per hour was designed and fabricated. A sheath of air, surrounding the primary coal and air stream, was used to prevent entry of hot gases from recirculating combustion products. Furnace temperatures needed for ignition ranged from about 1,8300 F for an Illinois coal to 2,250° F for a Beckley seam coal. Apparent flame velocities were about 2 to 5 feet per second, increasing with volatile content of the coal and with distance from the burner mouth to the flame. The time required for ignition, approximately 0.02 to 0.07 sec, was a better measure of flame behavior than was velocity.

Jan 1, 1969

By R. F. Abernethy

Analytical results, including ash fusibility data, are presented by the Bureau of Mines for 10 major constituents in coal ash from 373 samples of commercial U.S. coals. Determinations of Si02, Al2O3, Fe2O3, and P2O5 were made by colorimetric methods, Na2O and K2O by flame photometry, Ti02, CaO, and MgO by a spectrochemical method, and SO3 by a gravimetric method. In bituminous coal ashes the silicon, aluminum, and iron calculated as oxides often make up about 90 percent of the ash.

Jan 1, 1969

By Charles Prasky

The Bureau of Mines investigated the conversion of nonmagnetic iron minerals to magnetic form through reduction Toasting operations. The primary objective was to obtain a concentrate that could be used as a direct shipping material for blast furnace consumption. Crude iron materials from the Steep Rock Lakes, Ontario, area were prepared into a blend of 8 parts siliceous ore, 3 parts pyritic ore, and 1 part tailings. Experimental work included laboratory reduction roasting tests, two continuous 10-day campaigns, and one 12-hour test all in a 34-inch by 36¬-foot rotary kiln. The objective of the project was achieved in producing an iron concentrate containing about 66 percent iron with over 90 percent iron recovery. Desirable operating conditions were developed in the kiln but optimum process variables were not completely established.

Jan 1, 1969

By T. E. Hill

The Bureau of Mines investigated the possibility of physically separating Missouri and Minnesota granites into commercially usable fractions of feldspar, quartz, and mica by mineral dressing techniques. The probability of r covering a feldspar fraction from raw granite suitable for commercial uses was developed through correlation of the iron oxide content by extensive petrographic studies. This probability evaluation also included Wisconsin granites and a high-feldspar iron ore concentration tailing from Missouri. Laboratory recoveries of feldspar and quartz were on the order of 80 percent. Mineral content of each fraction was generally over 95 percent, indicating excellent response to separatory techniques, Acid leaching of feldspar and quartz concentrates to remove iron oxide improved the grades chemically; however, occluded iron oxide particles in the leached products prevented attaining top grades of feldspar. Mica was removed as scrap grade at low recoveries. Each concentrate conformed to some category of commercial feldspar, quartz, or mica.

Jan 1, 1969

By John M. Gomes

The preparation of tungsten carbide by molten-salt electrolysis was investigated. Sodium tungstate in the electrolyte and carbon from the graphite anode were the source materials, Optimum results were obtained with an electrolyte consisting of 83 mole-percent sodium chloride and 5.7 mole-percent each of sodium tungstate, sodium metaborate, and sodium hydroxide; a temperature of 1,000° to 1,025° C; an anode current density of 37 amp/dm2 or less; and an initial cathode current density of 150 amp/dm2. The yield was approximately 0.45 g/amp hr. The electrolytic tungsten carbide product contained approximately 5.4 weight-percent combined carbon as compared to 6.1 weight-percent for pure tungsten carbide. Microhardness of the electrolytic tungsten carbide, determined with a 50-gram load, varied from 3,480 to 3,970 dph. The material was friable and could be ground in a laboratory ball mill to less than 400-mesh particle size.

Jan 1, 1969

By K. R. Dorman

To further investigate the potential of precast concrete sets as a support medium for underground mines, the Bureau of Mines designed a five-piece precast concrete drift set for a small opening and tested it to destruction in a straining frame. Twenty-seven tests were made with three sizes of members using three loading conditions. In addition, six tests were made with sets in a distorted configuration, Test results and typical failure patterns are presented. A comparison of results with those previously reported for the three-piece set shows the five-piece set supports considerably larger total loads than does the three-piece set of equivalent cross section designed for the same size of opening. Recommendations are made for improvements in design.

Jan 1, 1969

By J. P. McGee

A 1,000-hour test with a gas turbine at 1,200° F showed a working fluid of 1 gr of ash per 100 scf of power gas (79 percent of the ash 7 to 35 microns in diameter) to be excessive for acceptable blade wear for commercial practicability. Blades in the turbine consisted of about 20 percent each of chromium, cobalt, and nickel; 3 percent molybdenum; 2-1/2 percent tungsten; and smaller amounts of manganese, columbium, and tantalum. Erosion of both the fronts and backs of the turbine nozzles was particularly heavy, the trailing edges being worn to a featheredge. Erosion of the buckets was less marked, although the leading edges were somewhat pitted. A refractory-lined combustor performed efficiently and with little abrasion of the lining by the ash-laden gas.

Jan 1, 1969

By J. T. McCartney

The Bureau of Mines has developed an automated reflectance scanning microscope system, primarily for determination of volume proportions, size distribution, and mode of association of the physical (petrographic) components of coals. The process, which is potentially more rapid and objective and less tedious than a visual microscopic procedure, involves magnetic tape recording of several millions of reflectance readings on micro-meter sized areas of polished coal surface and computer analysis and interpretation of some characteristics of the coal components. The system was tested in a study of pyrite distribution in steam coals. The application was essentially successful, but defects in polished pyrite surface characteristics and problems in adequate sampling prevented completely satisfactory results. Pyrite con-tent and coal-pyrite particle association could be determined nearly as well as by visual microscopy, but size distribution data were less acceptable.

Jan 1, 1969

By H. F. Feldmann

This Bureau of Mines report presents a method for the computer solution of the equilibrium compositions of any complex, multiphase, chemical system for which appropriate thermodynamic data are available. The method describes in detail the computation of systems in which solid or liquid species can form by heterogeneous chemical reactions where these species do not occur in any equilibrium equations. Also described are the calculation of phases formed by condensation (pure or solutions) and the inclusion of other system restrictions such as electroneutrality. The method is being used to compute the equilibrium composition of mixtures of an electrically conductive plasma and a liquid slag phase arising from the high-temperature combustion of coal for magnetohydrodynamic power generation. These mixtures can contain up to 65 species including gases, liquids, free electrons, and ions.

Jan 1, 1969

By R. E. Siemens

The Bureau of Mines sought to correlate the variation of structure-sensitive superconducting properties with microstructure in selected Cb-Hf alloys and to compare the experimental results with those predicted by the GLAG theory. Alloys in wire and rod form were evaluated by critical temperature, critical current, magnetization, resistivity measurements, and optical and electron microscopy. In the absence of an external magnetic field, the current carrying capacity of columbium was greatly reduced with addition of up to 85 wt pct Hf, but a large increase in Ic occurred for Cb-90 wt pct Hf. Favorable Ic-H behavior was observed in cold-drawn alloys containing 25 and 57 wt pct Hf. Correspondingly, a maximum in Tc occurred at 10-25 and 90 wt pct Hf. Four- or five-hour heat treatment at 600° C resulted in maximum Ic values and maximum hysteresis in magnetization. Dislocation pileup, polygonization, and fine precipitates, responsible for flux pinning, are listed in order of their effectiveness as pinning sites. Sites having an average separation of 1,500 to 3,000 A and a diameter of 1,000 A or less were most effective in influencing Ic-H and M-H behavior. The resistive critical fields increased smoothly to a maximum of 80 k0e between 60 and 65 wt pct Hf. Highfield, mixed state, reversible paramagnetism was observed in some alloys; however, the GLAG theory was in good agreement with experimental results for the majority of the composition range studied.

Jan 1, 1969

By W. E. Wallace

Volume-rate-of-flow measurements were made of the flow of mercury through porous samples under conditions of no field, magnetic field transverse to the direction of flow, and transverse magnetic field and electric current to determine if a magnetic method might be potentially useful in the study of pore-size distribution. No change was observed in the flow rate from the application of a magnetic field alone. The application of both field and current produced an electromagnetic pumping action with or against the direction of flow, depending upon the direction of the electric current. This pumping effect was observed to be greater in a rectangular porcelain sample than the calculated value for an equal-Sized open channel.

Jan 1, 1969

By G. H. Keith

The Bureau of Mines determined the mechanism(s) involved in observed anomalous changes in mechanical properties of vanadium-base alloys. Tensile properties of electrorefined and commercial-purity vanadium-base alloys containing up to 5 atomic percent molybdenum or titanium were measured between 77° and 673° K. Snoek oxygen and nitrogen peak heights were measured to determine the changes in dissolved interstitial content caused by increasing quantities of solute. In addition, changes in lattice parameter were followed wit: precision X-ray techniques. Softening, observed in alloys containing titanium, is explained by the formation of a second-phase titanium compound with oxygen or nitrogen. However, because of partitioning of titanium between compound formation and solid solution formation, about five times the stoichiometric amount was required for complete reaction. Addition of 1 percent titanium drastically lowered the strengthening due to strain aging, at 673° K, and 2 percent titanium essentially eliminated it. All alloys were ductile at 77° K. Variations in the tensile properties of the molybdenum-containing alloys are explained by variations in the amounts of interstitial impurities present. The molybdenum did not react with these impurities and had no effect on strengthening due to strain aging. Commercial-purity vanadium alloys containing more than 2 percent molybdenum were brittle at 77° K.

Jan 1, 1969