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By Thomas J. Blalock

The volumetric determination of uranium according to the method of Sill and Peterson (6),3/ which uses cerate oxidimetry after the separation of interferences such as sulfides and cupferrates, has been used for some time by the Bureau of Mines and gives satisfactory results for many of the samples tested. However, in those instances where the uranium content did not exceed a few tenths of 1 percent and iron was present in the range of 10 to 40 percent (as Fe203),4/ the method was cumbersome and unreliable. The need for a more accurate procedure for the determination of small amounts of uranium in the presence of large amounts of iron, such as in shale or black sands, prompted this investigation. The Bureau desired that materials containing as little as 60 p.p.m. of uranium be assayed within reasonable limits of accuracy. One of the primary aims of this work has been to eliminate, as far as possible, the necessity for repeated cup ferron extractions.

Jan 1, 1960

By J. Croeni

The search for new alloys for application in the atomic energy field had prompted investigation of zirconium-rare earth metal alloys by the Federal Bureau of Mines. In this instance the zirconium-dysprosium system was investigated by melting point, thermal analysis, resistivity, X-ray and metallographic methods. Results indicate a single eutectic system with a peritectoid reaction occurring at 890° C. The eutectic isotherm extends from 30 to 95-percent dysprosium at 1,280° C. Eutectic composition is located at approximately 70 percent dysprosium. Solid solubility of dysprosium in both alpha and beta zirconium is extensive. The extent of solid solubility of zirconium in dysprosium has not been determined. Although zirconium rich alloys exhibit a significant increase in hardness, they can be cold worked extensively. These alloys also appear adaptable to solution heat treatment. Additional investigations concerning corrosion resistance and other mechanical properties are necessary for satisfactory evaluation of these alloys. The superior corrosion resistance of zirconium and the nuclear cross-section characteristics of the rare earth metals have stimulated alloy investigations using zirconium as a base metal. Alloys combining these characteristics present a possible substitute for hafnium as a control rod material. In this particular study dysprosium was chosen as the alloying element, and several series of alloys were used to establish the equilibrium diagram.

Jan 1, 1960

By H. L. Gibbs

Many factors contributed to the decision to build a radiochemical laboratory at the Salt Lake City Metallurgy Research Center to investigate the application of radioactive isotopes and chemical compounds in extractive metallurgy. These reasons included the notable success achieved in biological sciences with radioisotopes, the development of reliable instruments and methods for identifying the isotopes and measuring their activities, and the commercial availability of radioisotopes in a variety of forms and known activities. The paramount reason, however, was the realization that better methods were needed for guiding and quantifying research to resolve the complex extractive metallurgy problems under study at the Research Center. This is the first of a series of reports describing the application of radioisotopes and radioactivity techniques in extractive metallurgy. The report includes a discussion of licensing and safety requirements, a general description of the laboratory and the methods used, a definition of the nature and scope of the research program, and a synopsis of the more important problems studied. Subsequent reports will concern radioactive techniques for solving specific problems in mineral dressing, hydrometallurgy, and pyrometallurgy.

Jan 1, 1960

By Walter Kawa

In connection with its research in producing synthetic liquid fuels from coal, the Federal Bureau of Mines studied reactions of iron and iron compounds with hydrogen and hydrogen sulfide in batch autoclaves. The Bureau hoped to gain indirect evidence regarding the chemical changes that iron catalysts undergo when they are used in the hydrogenation of coal. The information obtained may be helpful in identifying the active form or forms of iron catalysts. At 450° C., with hydrogen at hundreds of atmospheres and hydrogen sulfide at 1 or 2 atmospheres, the thermodynamically stable form of iron is ferrous sulfide in the case of the metal, magnetite, ferric oxide, ferrous sulfate, ferrous oxalate, or the chlorides of iron. However, complete conversion to ferrous sulfide was not achieved at temperatures of 400° to 500° C. for kinetic reasons. Extensive sulfiding of iron, magnetite, ferric oxide, and ferrous oxalate occurred below 400° C., and some conversion of ferrous sulfate to ferrous sulfide occurred at 400° C. In the hydrogenation of coal, ferrous sulfide is the form of iron likely to be available for heterogeneous catalysis when starting with the metal, oxide, sulfate, or oxalate.

Jan 1, 1960

By J. B. Gayle

This investigation was conducted by the Federal Bureau of Mines to compare the selectivities of diverse flotation reagents and also of flotation and float-sink methods of separation. Flotation tests, using sodium chloride, an alcohol-type frothing agent, and a kerosine-pine oil mixture as reagents, were made on seven coking-coal samples representing four different beds. The results indicated equivalent selectivities relative to sulfur rejection when entrapment effects were minimized by recleaning the various products. Selectivities relative to ash rejection were also equivalent for some coals; for others, the selectivities of the reagents tended to increase in the order sodium chloride, alcohol-type frother, and kerosine-pine oil. Float-sink tests on these same coals generally gave results indicating better selectivities than those obtained in flotation tests at comparable levels of recovery.

Jan 1, 1960

By W. A. Stickney

As part of a Bureau of Mines program to investigate recovery of manganese (Mn) from low-grade materials, laboratory studies were made of four samples of mill rejects: Three from Montana and one from Peru. These studies demonstrated that certain mill-waste products can be a potential source of manganese. Both manganese oxide and carbonate minerals were recovered by flotation in an acid circuit with a fuel oil-tall oil emulsion as collector. Sintering) required to prepare a physically acceptable product, also was used as a method of beneficiation. In addition to being low-grade, some of the samples presented problems of intimate mineral association and complex textures.

Jan 1, 1960

By H. D. Hess

This report describes in detail a unique occurrence of fersmite, (Ca, Ce, Na) (Cb, Ti, Fe, Al)2 (0, OH, F)6, which occurs as small anhedral inclusions and intergrowths with a tantalum-free columbite found in the metamorphic complexes of Ravalli County, Mont. Chemical and crystallographic data along with the physical and optical properties agree in general with those given in the original description of fersmite from the Ural Mountains of Russia. X-ray diffraction data not given in the original description and more specific optical data have been determined. The Montana fersmite, now established as the second occurrence of this rare calcium-columbate mineral, was discovered during a routine Bureau of Mines mineralogical examination of a prospector's sample.

Jan 1, 1960

By W. A. Grosh

Records show that much of the lead produced in the Upper Mississippi Valley lead-zinc field was taken from natural openings along crevice systems at shallow horizons or at the surface. During the early history of the district, the shallow deposits were worked intensively; but in recent years the production of lead, except as a byproduct of deeper mining for zinc ores, has not been significant. Considering the methods of early mining, the character of mineralization, and the fact that galena can still be found on the surface of the old digging areas, it was reasoned that enough mineralization might remain on and above bedrock to permit, through the use of modern equipment and methods, economical re-treatment of surface material in the digging areas.

Jan 1, 1960

By W. H. Ode

Because trade increased among various nations after World War II, the Coal Committee of the Economic Commission for Europe established a Classification Working Party in 1949 to develop an International system for classifying coal. Although national classification systems existed, they had been developed in accordance with characteristics of domestic coals without reference to coals of other countries. Terms for describing similar or identical coals differed in each nation. This caused confusion in evaluating coals shipped in international trade and also hampered exchange of technical information on problems of coal utilization. Experts4/ participating in the classification project early in their work agreed that two systems should be formulated, one for the higher rank coals or so-called "hard" coals in European terminology and the other one for the lower rank coals, the latter designated mainly as brown coals and lignites in the various countries. Rank refers to the degree of metamorphism (progressive alteration) in the natural coalification series from lignite and brown coal to anthracite. The system for classification of hard coals was published late in 1956 as a document of the United Nations.5/ Results of a study for applying this system to American coals were published in 1958.6/

Jan 1, 1960

By M. D. Carver

This publication describes development by the Bureau of Mines of a quality evaluation procedure for certifying the adequacy of production lots of Kroll process zirconium sponge the Bureau had produced for reactor applications. After the procedure was devised, the next step was to apply it in controlling the quality of one-half million pounds of zirconium sponge com-prising 259 production lots, called blends, originating at the Metallurgy Research Center of the Bureau at Albany, Oreg. The Bureau concluded that the evaluation method developed was adequate and that by this method the zirconium blends having impurity levels or other property values outside specification limits were differentiated and thus were diverted from nuclear energy end uses. The research was performed under contract for the Bureau of Ships, Department of the Navy, and for the Atomic Energy Commission (AEC).

Jan 1, 1960

By I. L. Feld

This report describes an attrition-grinding process and equipment for grinding coarse kaolins to the 2-micron particle-size range. The research was undertaken by the Bureau of Mines to devise an acceptable method for converting coarse kaolins, such as paper-filler-grade clays, to paper-coating-grade clays, thereby increasing the value and extending the life of the southeastern paper-clay deposits. The attrition-grinding process is basically the intense agitation of a slurry composed of the material to be ground, a granular grinding medium, and a suspending fluid. This process gave better particle-size reduction than that obtained by several other grinding methods. Results of batch tests in 5-and 10-inch-diameter attrition grinders demonstrated that a coarse kaolin containing about 13 percent minus 2-micron, equivalent spherical diameter (e.s.d.) particles was readily ground to give a product with 88 percent minus 2-micron e.s.d. material. Power consumption was reasonable in view of the increased value of the ground material. Comparison of particle-size reduction with power-consumption data for the two units indicated that better performance was obtained with the larger machine.

Jan 1, 1960

By M. R. Geer

The cleaning of fine coal, particularly for metallurgical use, is receiving greater attention. An increase in the proportion of fine coal in the run-of-mine product has been created by changes in mining practice, and a concur-rent deterioration in the quality of the fines has occurred because of more widespread full-seam mining. These two factors, augmented by the depletion of premium beds of metallurgical coal in some areas and the resulting shift to "dirtier" beds, are providing the impetus for adoption of improved cleaning techniques. For example, froth flotation, which has been used for years in a few preparation plants, now is gaining more rapidly in acceptance. Similarly, the dense-medium cyclone, which is used widely in Europe for making difficult separations, recently has been introduced to the United States. Regardless of the cleaning process employed, the finer sizes of coal can be treated with maximum effectiveness only when they are removed from the run-of-mine product and treated separately. No present process can treat the full range of sizes together with complete effectiveness. Flotation is applicable only to the coal finer than a top size ranging between 14-and 48-mesh, and cyclones require removal of all material finer than 0.5 to 0.3 mm. from the feed. Thus, the trend toward more-effective cleaning of the fine coal imposes the attendant problem of fine screening. Whereas in the past there was little need to screen finer than about l/4-in., present developments indicate that fine screening will become increasingly prevalent.

Jan 1, 1960

By G. H. Martindill

Complex chemical and physical changes occurring during carbonization result in a heterogeneous system composed of gaseous, liquid, and solid phases, whose relative proportions and chemical compositions change constantly as temperature increases. Studies in which the participating variables are isolated and controlled should be useful in formulating the mechanism of coal carbonization. The most characteristic property of a coking coal is its ability to form a plastic mass at a certain stage of the carbonization process. During this period it is believed that fluidity of the coal influences the properties of the resultant coke. This report gives results of an investigation by the Federal Bureau of Mines of the influence of the maximum fluidity attained by the charge on the physical quality of the coke or char produced. As a first approach to the problem, researchers investigated high-melting-point pitches, which are relatively simple carbonaceous materials. The plastic properties of these pitches, prepared specially for this work, varied greatly; their fluidities, as measured by the Gieseler plastometer, covered most of the fluidity range characteristic of coking coals. Blending these pitches with increasing pro-portions of fine coke progressively reduced their fluidities. Coal-pitch and coal-coke blends also were treated; their fluidities were varied by changing their blending ratios. The various blends were carbonized in a small-scale carbonizer and the resistance of the carbonized residue (char) to abrasion was determined in a small-scale tumbler test, using the Roga drum.

Jan 1, 1960

By Mary F. Koehler

Interoxidic compounds, such as vanadates, have not been studied extensively in the field of thermodynamics. This is a report of three vanadates of sodium--metavanadate, pyrovanadate, and orthovanadate. Vanadates of other metals will be considered in future reports. The heats of formation at 298.15° K. of the three sodium vanadates (both from the oxides and from the elements) were derived from the results of sodium hydroxide solution calorimetry. Free energies of formation were obtained by combining heat and entropy values. The results support the conclusion that the three sodium vanadates were stable with respect to all possible decompositions in which vanadium retains its pentavalency.

Jan 1, 1960

By J. D. Ramsdell

The purpose of this investigation was to determine the effects of the impurities, oxygen, nitrogen, carbon, and iron (in low percentages) on the mechanical properties of electrolytic titanium. The strength and hardness of binary Ti-O, Ti-N, and Ti-C alloys are linear functions of alloy content in the composition range investigated. Compared to oxygen and carbon, nitro-gen is the most effective strengthener and hardener, followed by oxygen, then carbon. When the carbon concentration is above 0.10 percent, carbides are present, and strength and hardness are relatively unchanged. For equivalent hardness levels, Ti-Fe alloys are stronger than binary titanium alloys containing oxygen, nitrogen, or carbon. However, the strengthening is related to the presence of transformed beta in the structure.

Jan 1, 1960

By P. C. Good

To meet a growing need for thorium metal of high purity and amenability to fabrication, the Bureau of Mines devised a method for preparing thorium metal by the reduction of thorium tetrachloride. Thorium tetrachloride was prepared by chlorinating calcined thorium oxalate with carbon tetrachloride. The crude thorium tetrachloride, containing oxygen-bearing compounds, was purified by a double vacuum distillation at 800 to 900° C., and thorium metal was made in the form of a dense sponge by the reaction of metallic sodium or magnesium with thorium tetrachloride at 800° C. Vacuum arc melting was used to consolidate the sponge metal to ingot form for evaluation of its physical and chemical properties.

Jan 1, 1960

By H. S. Caldwell

This report describes work by the Bureau of Mines on the vacuum distilla¬tion of some of the more volatile metals such as cadmium, zinc, and magnesium from lead and tin. Evacuation within a distillation apparatus allows rapid diffusion of vapor away from the evaporation surface and prevents reaction of the vapor with residual gases. A reduction of pressure to several tenths of a millimeter makes possible practicable distillation rates, at temperatures for which the partial pressure of the metal vapor exceeds 10-3 atmosphere. The rate and selectivity of distillation depend primarily on the volatility and molal ratios of the alloy metals, and their chemical activity to each other. For very rapid evaporation or low concentration of the more volatile constituent, the rate is determined by the rate of diffusion of the evaporating metal, to the surface of the melt. Cadmium, zinc, magnesium, and tellurium were found to volatilize readily from both lead and tin. Tellurium appears to volatilize as an intermetallic compound rather than the pure metal. Antimony could not be removed from lead at 1,000° C.; the condensate was nearly all lead. Antimony, bismuth, and lead were removed from tin.

Jan 1, 1960

By J. L. Konchesky

The technical feasibility of gasifying powdered, noncoking, low-rank coal with steam in an externally heated tube has been demonstrated. The tube, 112 ft. of alloy-steel tubing shaped into a helix, served as an electrical conductor of electricity used for heating. The effects of the following variables were studied: Residence time of coal in reactor, average reaction temperature, steam concentration, and rank or geologic age of coal. Reaction pressure was maintained in the range 19-26 p.s.i.a. High carbon conversions and large yields of synthesis gas were obtained with low-rank coal. In one test, for example, about 88 pct. of the carbon in a subbituminous C coal was gasified at 1,910* F. with a residence time of 1 sec. The gas contained 58 pct. H2, 19 COD 15 CO, and 3 CH4; the yield was 30 cu. ft. (at 32' F. and 14.7 p.s.i.) of synthesis gas (CO + H2) per pound of dry coal.

Jan 1, 1960

By James M. Stuckey

In a search for improved methods of upgrading tar obtained by low-temperature carbonization of coal, monoethanolamine (MEA) was found to be effective in extracting tar acids from coal tar distillates derived from a subbitunwous and a lignite coal. Patch extractions showed that both yield and purity of the extracted acids improved with increasing volume ratios of monoethanolamine to tar acid, varied from 1:4 to 8:1. Yield improved, but purity decreased as the concentration of monoethanolamine was changed from 30 to 70 volume-percent, and as the concentration of tar acid in distillate was increased ad from 14 to 45 percent. In a continuous countercurrent extraction employing a double solvent (monoethanolamine and hexane) approximately 80 percent of the tar acids was extracted from 170° to 350° C. tar distillate when using 1.6:1 volume ratios of amine:tar acids. Tar acids isolated from his extract, although of improved purity, contained appreciable quantities of neutral oils and some tar bases. Aqueous monoethanolamine was not effective for extracting the last 10 to 15 percent of tar acids in 170° to 350° C. distillate oil from lignite coal. The highest yield of isolated tar acids and the best recovery of monoethanolamine were obtained by diluting the extract with water and saturating with C02. Some losses of solvent were encountered when aqueous monoethanolamine solutions were heated through decomposition of the amine with the liberation of ammonia.

Jan 1, 1960

By George L. Gates

This report presents is an evaluation by the Federal Bureau of Mines of the effect of clay-water, brine, and oil-base drilling fluids on the productivity of test wells drilled on the Umiat anticline in U.S. Naval Petroleum Reserve No. 4 in northern Alaska. Eleven, wells were drilled on the Umiat structure as part of the U.S. Navy's extensive exploration of the Reserve during 1944-53 to determine the possibilities for oil production. The Federal Geological Survey cooperated in the exploration program and has published a comprehensive report3/ on the geology of the area and case histories of the wells. The re¬port also includes the results of special studies by the Bureau in connection with the drilling and coring of well 9 with oil-base mud in hole and was the source of much of the information used in preparing this publication. Of the eleven wells, four were drilled with rotary tools and water-base mud (one of the water-base muds was an oil-in-water emulsion mud), five were drilled with cable tools with brine in the hole, one was drilled with cable tools with brine in the hole and later reamed with rotary tools and crude oil, and one was drilled with rotary tools and oil-base mud. Although all of the wells penetrated sandstones that contained oil and gas, some were productive and others were not. The latter two wells, one completed with crude oil in the hole (with some added brine) and the other with oil-base mud, had the greatest productive capacities. The wells drilled with cable tools and brine in the hole had lower productive capacities. In contrast, two of three wells completed with rotary methods and fresh-water drilling mud and the well com¬pleted with rotary and emulsion mud were unproductive.

Jan 1, 1960