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By F. R. Cattoir

The Federal Bureau of Mines refined chromium from an aqueous electrolytic process in molten sodium chloride-chromium chloride electrolytes. Oxygen and nitrogen contents were reduced by a factor of 10 to 40, but most other impurities were little changed. The product usually contained a little more iron than the feed. Since iron was entering the bath from the iron pot and the graphite liner at a nearly constant rate, contamination of the chromium deposits by it was more serious at low currents and deposition rates. A few runs in an iron cell with a nickel liner yielded chromium containing one half as much iron as the feed, but up to 1.5 pct. nickel. In all cases the anode feed lay in the bottom of the container, which itself was used as the anode connection. With a 12-in. cell, variations in applied voltage from 0.05 to 1.5, in current from less than 10 to over 100 a., and in initial cathode current densities from less than 100 to over 2,000 a./sq.ft. had little or no effect upon the analysis of the metal produced) except for iron content. Changes in bath analysis from 3 to 11 pct. chromium were also without effect. These changes did bring about large differences in the physical forms of the crystals obtained. The thick heavy crystals produced at low voltage and current contained voids which made them difficult to leach free of chlorides. Easiest to leach were the thin leaf-like crystals obtained at around 1 v.

Jan 1, 1960

By N. E. Hanna

As part of a program for improving, the safety of permissible explosives, the Federal Bureau of Mines has undertaken an investigation to establish the ability of sodium chloride to reduce the incendivity of permissible explosives to firedamp atmospheres. A motivating influence for this investigation has been the comparatively extensive experience of British and other European investigators, who used sodium chloride as a component of their permitted explosives (1, 5, 6 7).5/ In the United States research and development work of this type has been less extensive, although sodium chloride has been added to permissible explosives as a cooling agent (9) for many years. The results of the first phase of this investigation were presented in a previous paper (8), which established that adding up to 10 percent sodium chloride to permissible explosives reduces the likelihood of ignition of firedamp in the gallery test; however, the results were somewhat inconsistent, and the conclusions were qualified. Accordingly, the investigation was continued with a study of the effect of added sodium chloride as a function of the quantity added and of the particle size of the salt.

Jan 1, 1960

By R. V. Lundquist

A method was developed by the Federal Bureau of Mines for evaluating viscosity data from slurries obtained in leaching sinters from the lime soda sinter process for extracting alumina from aluminous silicates. The logarithm of the viscosity was observed to be a linear function with time. The slope of the plotted line provides a means for evaluating viscosity behavior in a lime soda sinter blurry and also a means for comparing gelation characteristics directly with other variables in the lime soda sinter process. This report presents one aspect of a continuing study by the Bureau of Mines on methods for treating siliceous aluminum ores. It is one of the many programs of the Bureau concerned with conservation, development, and use of our domestic minerals resources. Previous investigations of lime soda processes, both by the Bureau4-7/ and industrial concerns, have demonstrated that sintered materials containing CaO, Na2O, A1203, and S102 in various combinations exhibit a tendency to gel or set when mixed with water or other extraction solutions. Gelling prevents satisfactory recovery of alumina and in extreme cases prevents operation of an extraction plant.

Jan 1, 1960

By W. A. McKinney

A sample of oxidized copper ore from a large deposit located in Pinal County, Ariz., about 50 miles northeast of Tucson, was treated by the Federal Bureau of Mines in a small-scale continuous pilot plant by a procedure which comprised acid curing complemented by water leaching and countercurrent decantation washing in a series of drag classifiers. A feed was prepared by pugging minus 1/4-in, ore with concentrated sulfuric acid and about 10 pct, of eater, followed by curing in batches for about 24 hr. The cured ore was fed continuously to a leach drum, where it was mixed with advance solution from the countercurrent washing system to dissolve the sulfated copper. The pulp was thickened and washed in four Esperanza-type classifiers, using a flocculating agent to obtain rapid settling and thickening. The leached ore pulps thickened satisfactorily in the drag classifiers when about 0.8 lb. of a polyacrylamide flocculant per ton of dry feed was used. Clear overflow liquors were obtained, and classifier rake products containing about 60 pct. solids were produced, As much as 90 lb./hr. of ore was treated in the plant, with a recovery of 60 pct. of the total copper or 80 pct, of the acid-soluble copper when 2 tons of water per ton of feed was used in washing. The acid consumption was 4.3 lb./lb. of copper recovered. On the basis of the maximum feed rate employed and the effective pulp-settling area of the classifiers, a total of 1 sq. ft. of pool area was required per ton of dry feed per day for the thickening and washing operations. The washing efficiency in the test was 95 pct.

Jan 1, 1960

By S. L. Ausmus

The work covered in this report is a continuation of an earlier feasibility study by the Federal Bureau of Mines and points out improvements in the skull-melting method for casting reactive metals such as titanium, zirconium, and hafnium. Machined graphite molds with laminated sections can be reused many times. Large tube sections can be produced by spin casting. Graphite powder is the best expendable mold material, but binders for this use must be compounded carefully. The effects of current and furnace atmosphere on the dependent variables of the casting technique are shown. Because of developments in casting technology for titanium which eliminate the basic problems of melting and pouring the metal, opportunities for improvement in the method have increased. The mold material and gate and riser configurations require particular attention. The limits of application of the casting method have yet to be defined. New knowledge in anyone of these areas could result in marked improvements and simplifications in casting methods.

Jan 1, 1960

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