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By Van E. Shaw

Three comparatively simple, efficient, and rapid extraction methods for the dissolution of yttrium and rare-earth elements from a euxenite carbonate residue have been developed, using dilute sulfuric acid as the solvent. Extraction processes have resulted in yields of 98+ percent of the total rare-earth elements and yttrium contained in the residue and have given preliminary separation between the cerium-group and the yttrium-group rare-earth elements. Extraction procedures presented are: Procedure 1. -The recovery of total rare-earth elements and yttrium by a cold dilute sulfuric acid leach at a pH of 2.5. Procedure 2. -The recovery of yttrium and yttrium-group rare-earth elements by leaching with dilute sulfuric acid at 125° F. and a pH of 3.0, with subsequent recovery of the cerium-group rare-earth elements by a cold dilute sulfuric acid leach of the residue at a pH of 2.5. Procedure 3. -The recovery of the total rare-earth elements and yttrium by fractional leaching as in procedure 1, followed by boiling the sulfate solution, which precipitates the cerium-group rare-earth elements and leaves the yttrium-group rare-earth elements in solution.

Jan 1, 1959

By H. W. Sohns

A retort was constructed in which fine particles of shale, entrained in steam or other gaseous media, could be retorted at controlled temperatures and residence times and the effects of retorting variables upon quality and quantity of products could be determined. Studies of the effects of temperature upon products obtained from Green River (Piceance Creek Basin, Colo.) and Chattanooga (Tenn.) oil shales were completed. The feasibility of using the retort to process a shale of extremely high moisture content from Brazil also was investigated. Air was used as the entraining medium in a series of studies in which combustion of some of the products of retorting within the retort tube supplied a major portion of the process heat. In another series, shale oil from a conventional retort was cracked thermally to obtain data for comparison with results of retorting en-trained shale. In still another series the effects of rates of steam flow and solids feed upon rates of heat transfer from the furnace to the process stream were studied. Crushed quartz rather than oil shale was charged to the retort in this series. A study was begun in which raw shale was partly retorted, the products separated, and the partially retorted shale recharged to the retort. The shale was to have been recycled until it was completely retorted in an effort to improve oil yield by recycle retorting; however, the project was terminated before the investigation was completed.

Jan 1, 1959

By B. W. Naugle

This report describes the carbonizing properties of coals from the principal beds in Cambria County, Pa. Samples of coals from Upper and Lower Freeport and Upper and Lower Kittanning beds having estimated minable reserves of 50-million tons or more were studied by the Bureau of Mines. Cambria County coals rank either as medium-or low-volatile bituminous. A preparation study indicated that all coals tested in this county, except one sample from the Lower Freeport bed, were responsive to cleaning and would yield a product with satisfactory chemical properties for metallurgical coal. All coals tested from Cambria County yielded strong coke; however, they expand excessively when carbonized singly, and should be used only as minor constituents in metallurgical coking blends when carbonized in slot-type ovens.

Jan 1, 1959

By Robert L. Montgomery

Heats of solution of samarium (III) oxide and chloride in hydrochloric acid and of samarium (III) oxide, sulfate, and hydrated sulfate in sulfuric acid were measured. The heats of solution of this hygroscopic oxide are larger than those from the literature, probably because of more complete removal of water in the present study. From the literature value for the heat of combustion of samarium, the heats of formation of samarium (III) chloride and sulfate are -244.18 ± 0.41 and -928.5 ± 1.6 kcal./mole, respectively. The heat of hydration of the sulfate is -34.7 ± 1.0 kcal./mole. The heats of formation of other samarium com-pounds have been recalculated, using the new data.

Jan 1, 1959

By Farrel W. Lytle

Instrumental analysis has become an indispensable tool in research and production of the rare-earth elements. This development can be attributed mainly to a combination of two factors--the marked chemical similarity of the rare-earth elements, which excludes classical methods of analysis, and the speed and accuracy of instrumental-analysis techniques. With continued improvements in methods of producing high-purity rare-earth elements, keeping pace instrumentally is becoming much more difficult. Accordingly, greater emphasis is being placed on improving instrumental limits of detection and accuracy. The methods employed most frequently for determining impurities in rare-earth elements involve use of the optical-emission spectrograph (3, 4)4/ and the spectrophotometer (9). Although numerous X-ray-emission spectrographic methods (6-8) have been developed for analyzing rare earths, these techniques have not included detection of low-level impurities. This investigation was conducted to find the precision and accuracy of X-ray fluorescence in deter-mining impurities in rare-earth oxides in the 0.01-to 1.0-percent-concentration range.

Jan 1, 1959

By W. H. Oppelt

A lignite from west-central North Dakota (Mercer County) was dried by the Bureau of Mines by the Fleissner process at saturated steam pressures to 1,500 pounds per square inch absolute (p.s.i.a.). Normally, the process is operated at pressures of 200 to 370 p.s.i.a. At the highest pressure the temperature of the saturated stearn is 596° F. The purpose of the investigation was to evaluate the influence of very high stearn pressure and temperature on moisture removal, steam consumption, and physical and chemical characteristics of the dried lignite. Two drying cycles were used: A normal cycle, corresponding to previously established standard time requirements, and an accelerated cycle, wherein time requirements were determined by boiler capacity and handling speed. Blank tests to determine stearn requirements for heating the empty autoclave were performed for each cycle and each test condition. Moisture removal, final moisture content, net steam consumption, and size stability of the dried lignite were determined.

Jan 1, 1959

By J. B. Gayle

Since the turn of this century, there has been increasing interest in the application of flotation processes to the beneficiation of finely divided minerals of various types, This is reflected by the large numbers of papers dealing with various aspects of this problem published annually both in this country and abroad. For the most part, such papers fall into one of three categories: 1. Those concerned with achieving, by various chemical and/or physical means, a set of conditions under which certain particles become potentially floatable while others do not. 2. Descriptive studies of plants and pilot plants effecting separations between such particles. 3. Studies of the effects of certain design and operating variables on the rates and efficiencies with which such separations can be effected.

Jan 1, 1959

By Alla D. Mah

The work described in this report is part of a Bureau of Mines research program for obtaining heats of formation of inorganic oxides, carbides, and nitrides by combustion calorimetry. The heats of combustion of molybdenum subnitride (Mo2N) and chromium subnitride (Cr2N) were measured. The data were combined with previous determinations of the heats of formation of molybdenum trioxide and chromium sesquioxide to obtain the heats of formation of the two subnitrides from the elements at 298.15° K. The corresponding free energies of formation were estimated. The heat data were compared with those of nine previously studied nitrides.

Jan 1, 1960

By S. L. May

The Bureau of Mines has developed several methods for extracting tantalum and columbium (niobium) and the rare-earth compounds from ores and concentrates. A cooperative agreement was made by the Bureau with Porter Bros. Corporation of Idaho to process 200 pounds of its euxenite concentrate by methods that had been developed at the Albany, Oreg., Metallurgy Research Center. The euxenite concentrate was processed to extract and purify the valuable metals by chlorination, solvent extraction, and hydrometallurgical techniques. Chlorination was used to convert the valuable constituents into chlorides and to partly separate them. Solvent extraction techniques were used to separate the tantalum from the columbium. The rare-earth and uranium compounds were purified by hydrometallurgical methods.

Jan 1, 1959

By H. C. Carpenter

Data are presented comparing results obtained with 17 different catalysts in hydrogenating crude shale oil to gasoline in single-pass operation. A method is described for predicting the maximum yield of gasoline obtainable at constant pressure for each catalyst from results of a limited number of experiments at different temperatures. Operating variables have considerable influence on yields and properties of products. With most of the catalysts, at operating temperatures below 890° F. liquid yield exceeded 100 volume-percent. Above this temperature the volume of liquid product decreased rapidly. Maximum gasoline production in most instances was achieved at a temperature higher than that at which the maximum volume of liquid product was produced.

Jan 1, 1959

By John B. Goodman

This report summarizes the work done by the Koppers Company, Incorporated, in cooperation with the Bureau of Mines on the commercial evaluation of the primary low-temperature tars produced from Texas lignite in the Rockdale, Tex., plant of the Aluminum Company of America in conjunction with the Texas Power and Light Company. The interest of the Bureau of Mines in this project is twofold. First, through its cooperative agreement with the Texas Power and Light Company the Bureau has assisted in the technical design and practical operation of the prototype, externally heated, entrained-state carbonizer for producing char for electric-power production and for primary low-temperature tar. Second, the first successful operation of the prototype carbonizers employing the Bureau of Mines-Parry process on lignitic coal in 1953-54 led to the production of large quantities of primary lignitic tar, concerning which too little was known or had heretofore been published in this country.

Jan 1, 1959

By M. R. Geer

Traditionally, fine coal is more troublesome than the coarser sizes at every step of the coal-preparation process--screening, cleaning, dewatering, and drying. Therefore the present trend toward a higher proportion of fines in the run-of-mine product, brought about by changes in mining practice necessitated to increase productivity, has added greatly to the task of preparing coal for the market. One of the more difficult and costly problems involved is that of recovering fine solids from the washery water. These fine solids should be recovered in the interest of conservation, and they must be removed to provide recirculating water of proper quality. If there is a plant effluent, it must meet increasingly stringent requirements against stream pollution. Vacuum filtration has been used for years at a few plants to recover the extreme fines, but its additional cost discouraged general adoption until recently. Now, with growing emphasis on better solids recovery, filtration is becoming more widespread. Many coal slurries filter readily, giving high cake rates and clean filtrates. Others, however, particularly those containing either a high proportion of material finer than 200-mesh or an appreciable amount of clay, are much more difficult to filter. Many of these refractory slurries can be rendered more filterable by flocculation. A previous report of Bureau of Mines research dealing with flocculation alone was published in 1940.5/

Jan 1, 1959

By D. J. Bauer

This report covers a phase of an extraction project carried out as part of a research program on rare-earth technology. The current project--the production of pure cerium compounds--is an intermediate step between ore processing and metal reduction. In this connection, a study on a separatory-funne1 scale was made on nonreducing extractants for recovering cerium (IV) from tri-n-butyl phosphate (TBP) and of methods for recovering the cerium nitrate from the strip solution. Dilute sulfuric acid was found to be 100 percent effective in stripping cerium (IV). Several precipitants were effective in recovering the cerium from the strip solution, and ethanol was especially promising. A scaled-up investigation was made into the use of spray-tower type equipment to perform the function of extracting, washing, and stripping. This equipment, referred to as the pressure-bubbler, utilized the system developed on the separatory-funnel scale. Feed solutions were prepared from a bastnasite concentrate by two techniques. Of these, the sulfated bastnasite solution was most successful, resulting in 86-percent recovery of the cerium at 99.7+-percent purity.

Jan 1, 1959

By J. E. Wilson

The Pittsburgh carbonization laboratory of the Bureau of Mines has determined the expansion or contraction of more than 300 coking coals in a modified Bethlehem-type sole-heated expansion tester. Information on the actions of coals or blends of coals when coked is extremely valuable to operators of commercial-scale coke ovens. Coals that expand abnormally or beyond expectations can cause extensive damage to coke ovens and result in costly shutdowns and repairs. Although test results for many of the coals have been given in various Bureau of Mines publications, considerable information was not published. Thus, it is the purpose of this report to furnish coal operators and the coking industry with a current appraisal of the expanding properties of all coals tested by the Bureau before September 1, 1958. These data should be useful in the normal long range planning of coal and coke production and will be essential if the demand for coking coals increases abnormally or when reserves of higher grade coals are depleted.

Jan 1, 1959

By William J. Campbell

These investigations were undertaken as part of a program to determine the optimum X-ray spectral lines to use for analyzing the wide variety of samples received by the X-ray Laboratory. Theoretical calculations and experimental data derived from these investigations show that longer wavelength spectral lines, > 2A, are very useful for many analytical problems. Because of the low fluorescence yield of the elements of atomic numbers 13-22 and the small depth of penetration of their X-ray spectral lines, these elements were originally considered to be insensitive; however, these studies show that the wide dispersion of their spectral lines, coupled with their weak beta lines, permits the use of wide collimation, thus increasing the line intensity. More importantly, the background due to scattered primary radiation is very low in the long-wavelength region.

Jan 1, 1959

By V. A. Nieberlein

Problems of design involving the high-temperature characteristics of materials of construction have focused attention on tungsten, the metal with the highest melting point. To study the properties of this metal a method was needed to produce tungsten of high purity easily and consistently. The Bureau of Mines has made tungsten metal in massive form on a laboratory scale by hydrogen reduction of tungsten hexafluoride (WF6). Metal made in this manner had a purity of 99.99 percent or better, with reference to all detectable impurities, including gases. The process tolerated a wide variation in operating conditions, and the results with respect to total impurities as low as 0.01 percent were reproducible.

Jan 1, 1959

By A. C. Rice

This report describes a chemical process for preparing solutions of trivalent rare-earth chlorides from sulfate solutions obtained by treating bastnasite concentrate. The chief impurity in the final solution is cerium, and this element is less than 1 percent of the rare-earth oxides. The solution is used directly in the separation of rare-earth elements by ion-exchange methods. The attractive features of the process are that the chemicals are inexpensive and the steps few. The process starts with precipitating the rare-earth hydroxides from sulfate solutions with caustic soda. After the hydroxides are dried to oxidize the cerium, they are treated with dilute hydrochloric acid to dissolve away the trivalent rare-earth elements, leaving the tetravalent cerium. Details for controlling the leaching step are described. The process shortens older procedures by omitting the usual oxalate or double-sulfate-precipitation step.

Jan 1, 1959

By R. M. Jimeson

Pressure-drop measurements through beds of granular iron, lathe turnings, steel wool, and parallel-plate assemblies were made at linear velocity and gas-density ranges expected in the Fischer-Tropsch hot gas recycle process.4/ Equations relating pressure drop, linear velocity, gas density, and bed porosity were derived. The results indicate that the exothermic heat of reaction can be removed at a lower cost by using catalyst beds with high porosity. INTRODUCTION The Fischer-Tropsch hot-gas-recycle process requires a catalyst offering low resistance to gas flow as one condition to economic feasibility. Conventional granular or spherical catalysts used during early development of the process in Germany did not meet this requirement. Large pressure drops across these beds made the cost of recirculating the gas excessive. The Federal Bureau of Mines is investigating the process by using novel and unusual catalysts that offer little resistance to gas flow. Pressure-drop measurements across these types of catalyst beds are discussed in this report.

Jan 1, 1959

By Foster Fraas

Almost all minerals show irreversible changes in electrical conductivity after heating in the temperature range 100° to 800° C. This effect can be detected with only a limited number of minerals with the standard ionizing-electrode-type separator, which differentiates between nonconductors and conductors in the single-particle resistivity range of 1011 to 1013 ohms. Tests outside this range with other type separators, such as the static field type, increase the number of minerals with which the effect can be detected to almost all that were tested. Irreversibility may be the result of an alteration of adsorption layers, volatilization of surface cations or anions, or an oxidation or reduction. One example is limonite, which decomposes to hematite and passes through two minima and two maxima in conductivity in the temperature range 100° to 900° C.

Jan 1, 1959

By M. J. Ferrante

A process was investigated for preparing Specification-grade nickel (containing less than 1 percent cobalt) by stripping it electrolytically from a nickel sulfate-boric acid solution and using the stripped electrolyte for the preferential dissolution of nickel from basic carbonates of nickel and cobalt. The basic carbonates were produced at the plant at Nicaro, Cuba, owned by the U.S. Government. Determination of the optimum conditions for deposition of Specification-grade nickel indicated that the upper limit of cobalt concentration was 0.1 gram per liter. The pH, temperature, and concentrations of nickel and boric acid in the electrolyte were not critical. An aluminum cathode and two lead anodes were used at a cathode current density of 1.2 amperes per square decimeter.

Jan 1, 1959