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By R. L. Crosby

From studies of wrought magnesium alloys containing rare-earth elements, data are presented on the mechanical properties of the alloys at room temperature and at temperatures of 100°, 200°, and 300° C. Results of studies of the solid-solubility of cerium and zirconium in magnesium as determined by electrical resistance measurements are also discussed and are compared with those of other investigators. The strength of magnesium-cerium alloys did not increase with the addition of vanadium and titanium dioxide. The addition of zirconium increased the tensile strength of the alloys as much as 10,000 p.s.i. at room temperature, but this increase diminished above 100° C.

Jan 1, 1962

By J. G. Croeni

The titanium-iridium alloy system was investigated to determine whether alloys of this system would merit further development as control-rod material for nuclear reactors. A study was made to determine the titanium-iridium phase diagram by using melting-point, thermal analyses, X-ray diffraction, dilatometric, electrical resistivity, and metallographic techniques. The titanium-iridium alloy system was investigated between 500° and 2,400° C. Results indicate the formation of two intermetallic compounds, Ti3Ir rind TiIr3, and one intermediate solid solution centered about the 50 atomic percent iridium composition. A eutectic reaction occurs at 1,475° C, and 19 atomic percent iridium. The Ti3Ir decomposes peritectically at 1,520° C. The intermediate solid solution exhibits a maxima of 2,140° C. at 50 atomic percent iridium. This phase is also believed to undergo an order-disorder transformation at 1,750° C. Another eutectic reaction takes place at 2,000" C. and 60 atomic percent iridium. The compound TiIr3 formed at 75 atomic percent iridium decomposes peritectically at 2,115° C. Further increases in iridium content result in the formation of an iridium-rich terminal solid solution. Information obtained below 900° C. in titanium-rich alloys indicates that iridium acts as a beta stabilizer in titanium, and the authors believe that a eutectoid decomposition of beta-titanium occurs near 500° C. and 10 atomic percent iridium.

Jan 1, 1962

By T. T. Campbell

Research conducted by the Bureau of Mines demonstrated the feasibility of preparing columbium and tantalum metals by the application of Kroll-process techniques. Yields in excess of 95 percent were obtained in a modified Kroll-process reduction apparatus constructed from nickel and Inconel.4 Operating conditions during reduction and distillation were determined. Optimum temperatures during sodium reductions ranged from 650° to 750° C and for magnesium from 700° to 800° C with retort pressures ranging from 3 to 7 psig. Undesirable vapor phase reactions occurred when temperatures exceeded 750° C during sodium reductions or 850° C with magnesium. Vacuum distillation at 850° C effectively removed volatile salts and excess reductant from the reduced metals. Calculations based on the results obtained in small scale tests indicate that reaction rates of up to 34 lb/hr could be obtained during columbium reductions and up to 60 lb/hr during tantalum reductions in production scale reac¬tors. The small, laboratory-scale techniques used in this study could be adapted to commercial practice. The reduced powder or sponge metals can be consolidated by conventional arc-melting techniques, and the arc-melted metals can be fabricated into ductile sheet at room temperature. Analyses of arc-melted buttons prepared from Kroll-process tantalum or columbium showed that tantalum of greater than 99.8-percent purity was obtained and that columbium purity exceeded 99.7 percent. A significant purification of the reduced metals occurred when they were consolidated by electron-beam melting, and the purity and ductility of electron-beam-melted Kroll-process tantalum and columbium compared favorably with the commercial metals. After electron-beam melting, the purity of the tantalum exceeded 99.95 percent, and columbium purity was approximately 99.9 percent.

Jan 1, 1962

By P. A. Wasson

Drill cores from 15 holes in the West Central Mesabi Range were studied as part of the Lake Superior iron resource investigation begun in 1957 by the Bureau of Mines. Chemical, petrographic, and metallurgical analyses were made to determine grade, mineralogy, magnetic characteristics, and response to beneficiation. Data in this report were developed to provide a better under-standing of the nature and character of low-grade iron ore occurrences, to measure potential of usable ore, and to provide a basis for comparison with bank samples previously taken in the same general area. The average iron content of 4,445 feet of core was 31.8 percent. Iron oxides present were hematite, goethite, and magnetite; the gangue minerals were chiefly quartz, iron silicate, and iron-bearing carbonates.

Jan 1, 1962

By W. A. Calhoun

A method for concentration of the nickel-cobalt-bearing mineral, siegenite, from a table middling has been developed by the Bureau of Mines at Rolla, Mo. The table middling is composed of a complex series of sulfide minerals, occurring in mill operations in the southeast Missouri "lead belt." In these operations the siegenite is lost as a separate concentrate, being diverted to other products. The procedure also includes recovering commercial-grade concentrates of copper and lead. A low-grade zinc concentrate, a potential coproduct, was also made.

Jan 1, 1962

By R. C. Corey

Anticipating the need for convenient, economical, and safe means for disposing of combustible wastes contaminated with low-level activity, in connection with private and institutional uses of radioisotopes, the Atomic Energy Commission (AEC) has provided the Bureau of Mines with funds to develop an incinerator for this purpose. A prototype incinerator, designated hereafter as BOMAEC-30, was designed, constructed, and tested, based on fundamental and applied research investigations of the combustion characteristics of rubbish and sawdust, which will comprise the bulk of contaminated wastes. No radioisotopes were used in the tests; the objective was to remove as much particulate matter from the products of combustion as possible. The prototype unit was designed to burn 30 pounds per hour, using 100 percent over fire air admitted tangentially in an all-metal, cylindrical combustion chamber. The gas-cleaning system consisted of special fabric bags and absolute filters.

Jan 1, 1962

By J. W. Montoya

The chemical, mineralogical, and physical properties of berylliferous tuff from Spor Mountain, Utah, were determined in laboratory research conducted by the Bureau of Mines. Two beryllium-bearing minerals--a hydrated form of bertrandite and a berylliferous saponite--were found to be present in the tuff. Each of the beryllium mineral forms predominated in samples from certain areas of the district. The possibility of practicably separating the beryllium minerals from the tuff by physical methods appears remote because of the complexity and nature of the mineral associations. Beryllium mineralization in the region occurs in a rhyolitic tuff usually overlaid by unaltered rhyolite. The beryllium is distributed erratically throughout the tuff in individual mineralized bodies. Many samples of mineralized tuff were examined and found to contain from 0.2 to 1.8 percent BeO. All samples contained a hydrated form of bertrandite that was nearly cryptocrystalline, whereas samples from one area also contained a berylliferous saponite of variable beryllium content. Neither mineral has been previously reported, although related bertrandite-like minerals have been found in the U.S.S.R. and berylliferous minerals of the montmorillonite group have been synthesized. Most of the minerals of the tuff are finely crystalline, intergrown, and have similar densities. The complexity and intimacy of the mineral associations, the difficulty of achieving effective mineral liberation, and the highly friable nature are characteristics that lead to the conviction that tuff of the type examined cannot be effectively concentrated by gravity, magnetic, electrostatic, attrition, washing, sizing, or flotation methods.

Jan 1, 1962

By G. H. Gronhovd

This report describes the design and initial operation of a slagging gasification pilot plant installed by the Bureau of Mines at the Lignite Research Laboratory, Grand Forks, N. Dak., in 1958-59. The tests covered in this report were conducted over a period of about 2 years, beginning in April 1959. The pilot plant was designed for eventual operation at pressures ranging from 400 to 600 p.s.i.g. (pounds per square inch gage); however, for the preliminary test reported here, the gasifier was fitted with a low-pressure slagging section and operated at atmospheric pressure and at 80 p.s.i.g. The reason for using a low-pressure slagging section for initial operation was to facilitate modifications in design during the development of a reliable slagging procedure.

Jan 1, 1962

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1962

By A. Gene Collins

During recent years the interest in trace and minor constituents of oil-field water, petroleum, and their associated reservoir rocks has increased. The metals copper, nickel, lead, manganese, iron, zinc, and cadmium are not determined routinely in oilfield brine analyses. Determination of these metals and subsequent correlation of these data should yield information to aid 1n the interpretation of the origin of different waters. The methods of analyzing oilfield waters have several potential applications: (1) Aiding in the search for petroleum; (2) identifying sources of intrusive brines; (3) controlling corrosion; (4) controlling produced water; increasing knowledge of the geology of subsurface formations; (5) identifying incompatible waters in waterflooding operations; (6) increasing the knowledge of the flow of oil, gas, and water in underground formations; and (7) aiding in the identification and location of valuable mineral reserves. Some brines contain enough valuable minerals to be recovered commercially.

Jan 1, 1962

By Foster Fraas

A method is presented for the linear evaluation of adsorption data using the equations dC = Ae-rv dv and v = [jT] - q, where dC is the phase composition increment, v a calculated parameter, T the absolute temperature, and A, r, h, g, and q the constants. The value of v is calculated from the composition C for both the adsorption surface and the immersion phase. A plot of v for each phase on Cartesian coordinates results in straight line graphs. With temperature variation, a plot of v versus,[ ] also results in straight line graphs. The equations are applicable to electronic and salt equilibria.

Jan 1, 1962

By Sidney Katell

This report is an economic evaluation of the production of hydrogen in a continuous system by the steam oxidation of partially reduced iron oxide in a fluidized bed at 7 atmospheres using producer gas to reduce the iron oxide. The oxidation-reduction step is based on experimental data obtained by the Bureau of Mines at the Pittsburgh Coal Research Center. The estimated capital requirement for a plant producing 30 million std. c.f.d.3 of 99.8 percent purity hydrogen at a discharge pressure of 450 p.s.i.g. is $13,100,000, using January 1961 equipment cost data. Based on a 330-day operating year, the operating cost before profit and taxes with coal price as a variable is estimated to be:

Jan 1, 1962

By R. V. Lundquist

The work described in this report, part of the Bureau of Mines long-range program to develop methods of utilizing submarginal domestic sources of aluminum, was undertaken to investigate the effects of iron in the lime soda sinter process, The approximate Fe2O3 content in a sinter for maximum alumina and soda recovery was 8 to 9 percent. Fe2O3 appears to inhibit gelation, and 15.5 percent Fe2O3 produces effects similar to those produced by 1 percent sucrose. In the lime soda sinter process, aluminum silicates are sintered with limestone and soda ash to yield dicalcium silicate and sodium aluminate. The sodium aluminate is extracted by leaching in caustic solution. The solution is purified by heating in an autoclave with lime to remove silica, and alumina trihydrate is precipitated with carbon dioxide. The reactions involved in sintering and leaching are complex. A number of studies by the Bureau of Mines4-9 and others1 indicate that the iron content of sinters influenced the recovery of alumina and soda and the gelation characteristics.

Jan 1, 1962

By A. B. Whitehead

A spectrographic method for the determination of 18 impurities in cerium is presented. The carrier distillation technique is utilized to separate the spectra of impurities from the complex spectrum of cerium. Metal samples are ignited to the oxide, mixed with silver chloride carrier containing an internal standard, and excited with a 20-ampere direct-current arc. An additional exposure, made after carrier depletion, provides for the determination of refractory elements. Experiments to determine the best carrier, sample-carrier ratio, electrodes, arc current, exposure conditions, internal standards, and any matrix effect are described. The relative standard deviation of the method at the 20- and 200-part-per-million levels is about 25 and 15 percent, respectively. The average relative error is about 20 percent in the 10- to 1,000-part-per-million concentration range.

Jan 1, 1962

By H. E. Powell

A series of alkyl-dithiocarbamic acid amine salts was prepared and tested as collector for slimed lead minerals contained in the waste material from a commercial lead ore concentrator. The reagents, members of a homologous series differing only in the number of alkyl radicals in their structure, were prepared by reacting stoichiometric amounts of primary amines and carbon disulfide in a cold alcohol solution. Subsequent purification was by recrystallization from absolute ethyl alcohol solution. Evaluation was through froth flotation of a mill tailing containing 0.2 percent lead. Results show that maximum recovery (38 percent) was obtained with the reagent containing 8 alkyl radicals, but that maximum rougher concentrate grade (4.8 percent) was obtained with the reagents of intermediate number of radicals.

Jan 1, 1962

By Eliot J. White

The physical properties and clay mineral content of the major oil-producing formations in the Powder River Basin of Wyoming were determined by analyses of cores from 100 wells. Interrelationships were established among permeability, restored water saturation, clay content, and bulk swelling capacity of the crushed sample and used to estimate the susceptibility of the formations to water damage. The ratio of water permeability to gas permeability (kw/ki) offers a convenient scale for semiquantitatively estimating the water sensitivity of sands. The irreducible water saturation was also found to have a similar relationship to the clay mineral content and the water sensitivity of the sands. The average relation of water permeability to gas permeability is different for each sand, as shown by the curves, and the relative positions of the curves indicate the degree of water sensitivity of each sand from which the susceptibility to water damage may be estimated. How accurately these estimates show formation behavior under field operations will not be known until studies of field performance can be made. The water permeabilities of the Muddy, Minnelusa, and Tensleep sands average about the same as the gas permeabilities, and these sands are classified as insensitive. The water permeabilities of the Sussex and Shannon sands, at the other extreme, are much less than the gas permabilities [when average ki is 30 millidarcys (md), kw is 6.1 md], and these sands are classified as highly water sensitive. The sensitivities of the five other sands are between these extremes.

Jan 1, 1962

By George E. Fish

This report describes investigations conducted by the Bureau of Mines from 1957 through 1959 in the Roseland anorthosite-titanium belt of Nelson and Amherst Counties, Va., for the purpose of studying the titanium resources of the area. Three titanium deposits containing much saprolite ore derived from the decomposition of anorthosite and diorite were selected for detailed study Following a reconnaissance of the reported titanium occurrences in the belt. These three deposits occur in or are associated with anorthosite. Most of the occurrences are situated on or near the contact between the anorthosite and the gneissic country rock. The saprolite deposits are as much as 1.5 miles long, 1,000 feet wide, and 100 teat deep and contain significant reserves of titanium-bearing material estimated in excess of 20 million tons. Where it was penetrated by drilling, the unweathered rock beneath the saprolite contains nearly the same titanium values as the saprolite.

Jan 1, 1962

By M. E. Tyrrell

The purpose of the work leading to this report was two-fold: (1) To determine the properties of cemented tungsten carbide modified by the addition of one, two, and five percent of titanium diboride, and (2) to compare the properties of these mixtures when sintered, hot-pressed, and flash-welded (resistance-sintered). Minor additions of titanium diboride to mixtures of 94 percent WC and 6 percent Co decrease mechanical strength but increase oxidation resistance in proportion to the amount of the addition. One percent of titanium diboride increased the hardness by 2 Rockwell A units. Hot-pressing produced compacts with the highest density and the best mechanical strength, but losses of cobalt were high and grain growth was pronounced.

Jan 1, 1962

By C. J. Thompson

In the course of the work currently conducted by the Bureau of Mines in cooperation with the American Petroleum Institute Research Project 48 on identifying sulfur compounds in petroleum, a micromethod was developed (12)5 for catalytically removing the sulfur atom from sulfur compounds. The product is the residual portion of the molecule; the structure otherwise was unaltered except for hydrogenation of any unsaturated bonds that were present in the original compound. Positive identification of sulfur compounds isolated from crude oils is a difficult problem. Direct comparison of properties of the unknown with those of reference compounds is often impossible because of the limited number of reference sulfur compounds available. However, a relatively large number of pure hydrocarbons is available, and the conversion of the sulfur compound to a hydrocarbon enhances the possibility of identification. The technique also can be used to prepare microquantities of scarce hydrocarbons by hydrogenating compounds that are readily available.

Jan 1, 1962

By H. J. Seim

An ion-exchange-instrumental analysis technique is described for analyzing impurities at 1 to 1,000 parts per million level in rare-earth metals. A cation-exchange flame photometric method is used for the alkali and alkaline earth groups of metals, and an anion-exchange procedure is used in conjunction with polarographic and X-ray fluorescence techniques for selected transition elements. The standard deviation is about 6 percent, and the average error, about 5 percent.

Jan 1, 1962