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A spectrographic procedure applicable to the semiquantitative determination of 29 elements in tungsten is presented. The method is designed to give estimates of impurity concentrations up to 500 p.p.m. Limits of detectability range from 0.3 p.p.m. for the more sensitive elements to 100 p.p.m. for the less sensitive ones. Tungsten metal samples varying in particle size from minus 300-to 30-mesh are excited in the presence of 5 percent germanium with a direct current arc. Germanium acts to stabilize the arc, minimizes the volatilization of tungsten, and serves as an efficient carrier to sweep impurities from the tungsten into the excitation zone. Curves are presented that show the volatilization behavior of germanium, tungsten, and impurities in tungsten at different concentration levels. Data obtained were used as guides in establishing the method of analysis. In the absence of established reliable analytical procedures for determining many impurities in tungsten in the parts per million concentration range, the spectrographic method described here should prove to be helpful in evaluating high-purity tungsten.

Jan 1, 1961

By W. S. Landers

In contrast to the large fund of information available on the carbonizing properties of Eastern U.S. coals, the experimental data available for most Western U.S. and foreign coals are meager. To supply some self-consistent data, the Bureau of Mines conducted 220 low-temperature carbonization assay tests at 500° C. in a laboratory-scale carbonization apparatus. The results are included in this report. The U.S. coals tested are from Alaska, Arizona, Colorado, Illinois, Montana, New Mexico, North Dakota, Pennsylvania, Ohio, Texas, Utah, and Wyoming. Assays were also made on coals from Canada, Ecuador, France, Greece, India, Mexico, the Philippine Islands, Thailand, and Yugoslavia. In addition, one assay of pine sawdust and one assay of a peat from Ireland are reported. Prediction equations were developed relating the yield of products of carbonization obtained at 500° C. in the assay unit to the proximate and ultimate analyses of the coals. The equations for predicting the yields of tar plus light oil, char, and gas, and the heating value of the gas, are considered good, each equation having a multiple correlation coefficient of 0.90 or higher. The equation predicting volume of gas obtained upon carbonization is considered as fair, with a multiple correlation coefficient of 0.84. A reproducibility study of the assay made on 10 replicate samples of a subbituminous coal indicated that the standard deviation of the individual products was 0.31 percent or less.

Jan 1, 1961

By M. R. Geer

The washability examination of a coal establishes the quality of the product that could be prepared by mechanical cleaning, shows how much impurity would have to be eliminated to attain a particular quality of product, indicates what type of cleaning process would be suitable, and tells whether the coal could be cleaned efficiently, The coal-preparation laboratories of the Bureau of Mines make washability examinations of coal for a variety of purposes. Sometimes these examinations are made as an integral part of research conducted on coal-washing problems. Occasionally they are made on coals mined on Government-owned land or on coals destined for use in Government installations. Often they are made on coals from new fields or new beds in existing fields to help establish the characteristics of the Nation's coal reserves. Whatever the original reason for doing the work, the results often are useful later in evaluating deposits or in the design of cleaning plants. Publication of the results of such studies provides for the widest possible usefulness. This report brings together the results of washability examinations made on 1 coal each from Oregon and Idaho, 2 from Wyoming, 5 from Utah, and 11 from Washington. Material of this nature is inherently difficult to summarize. Some of the coals are so clean} despite full-scam mechanical mining, that they could not be improved materially by washing; others present some of the most difficult preparation problems found in the country.

Jan 1, 1961

By W. A. Cole

This report covers the preliminary phase of an investigation of clays, shales, and certain rocks in Wisconsin to determine the feasibility of processing lightweight aggregate in the State. The study was extended to include rotary-kiln testing of a limited number of shale samples, and to an appraisal of the Maquoketa shale resources in eastern Wisconsin. A total of 45 samples of clays, shales, and other argillaceous rocks of Wisconsin were tested. The lower Maquoketa shale is the only material found to date that offers possibilities as a source of material that can be processed in a rotary kiln for lightweight aggregate. Bedrock occurrences of the Maquoketa shale are found in the eastern and southwestern parts of the State. The populous southeastern region of Wisconsin presents a large potential marketing area for lightweight aggregate. For this reason special study was directed to the Maquoketa shale in the eastern district.

Jan 1, 1961

By W. M. Dressel

A simple field test for detecting the presence of germanium in rocks, coals, and flue dust has been developed by the Bureau of Mines. The method consists of dissolving germanium from the samples by either acid or fusion treatment methods, adding a few drops of hematein or phenylfluorone dye, and extracting the resulting colored complex with carbon tetrachloride. INTRODUCTION Germanium is obtained commercially as a byproduct of zinc production, as a coproduct of base-metal refining from germanium-bearing mineral, and as a recovered product from the ash of some coals. The growing use of germanium in the electronics industry has increased demand for this semiconducting metal to the extent that an intensive search for new sources of supply is necessary.

Jan 1, 1962

By Paul S. Lewis

Bench-scale experiment~ by the Bureau of Mines showed the gross effect of retention times ranging from 0.1 to 14.5 minutes on the conversion of high-volatile C bituminous coal to liquids and gases. The uncatalyzed coal was hydrogenated at 400°, 450°, and 538° C. and 500, 1,000, and 2,000 p.s.i.g. The percent coal conversion increased rapidly during the initial 3 minutes and asymptotically approached a maximum within 7 minutes at all conditions. Reasonably good correlations of coal conversion with time, pressure, and temperature were obtained. Temperatures up to 900° C. and retention times of about 1 minute are recommended for future experiments with the objective of producing only gaseous hydrocarbons and partially devolatilized coal suitable for use as solid fuel. The reactor contained 13 semicircular ledges, and the retention time was controlled by the rotation of scrapers which swept the coal from ledge to ledge. Only coal feeds that did not adhere to the internal mechanism could be used.

Jan 1, 1961

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Boone County, W. Va., as determined by the Bureau of Mines. It is one of a series describing the coals suitable for producing metallurgical coke, either as mined or after beneficiation. Over 6.3 million tons of coal was produced in Boone County, W. Va., in 1959, of which almost 5.5 million tons was mechanically cleaned in eight preparation plants. On December 31, 1959, it was estimated that almost 8 billion tons of coal remained in the county in beds 24 inches or more in thickness. Thirteen samples were collected from nine coalbeds and washability tests were made on these samples.

Jan 1, 1961

By William G. Gruzenaky

The separation of yttrium and the individual rare-earth elements (lanthanons) from mixtures in which they occur has been a difficult problem through-out the years. Because of the increased interest in the various uses of these metals, the economy of their production may become of great importance. Studies relative to this problem, undertaken at the Federal Bureau of Mines Albany Metallurgy Research Center, resulted in the development of a solvent extraction method by which yttrium can be separated from the rare-earth metals. A separation factor of 10.93 was obtained between yttrium and cerium from a single-stage extraction, and a factor of 1.78 was obtained between yttrium and erbium from a multistage system. The valuable metals were extracted from euxenite by caustic soda fusion or by chlorination, and several separation methods were investigated. Partial separation of the yttrium and rare-earth element fraction was made by chemical methods and by solvent extraction. Thermal decomposition of aqueous rare-earth nitrates or selective ignition of yttrium and rare-earth oxalates yielded a fraction enriched in cerium. A fraction enriched in the light rare-earth elements resulted from a double sulfate precipitation, whereas a potassium ferrocyanide pr cipitation yielded a fraction enriched in yttrium. Precipitation with dimethyl phosphate yielded a fraction enriched in yttrium and heavy rare-earth elements. Enriched fractions were obtained with several solvent extraction systems. A system consisting of rare-earth nitrates, nitric acid, and tri-n-butylamine-3 methyl-2-butanone favored the separation of yttrium from the heavy as well as from the light rare-earth elements.

Jan 1, 1961

By S. J. Gasior

Pilot plant studies showed the technical feasibility of fluidized-bed operation for producing hydrogen and synthesis gas by the steam-iron process. A mixture of iron and iron oxide from 20-to 100-mesh was partially reduced with a simulated producer gas and then oxidized with steam and/or carbon dioxide. Results of tests show the effects of pressure, temperature, bed height, gas-to-solids ratio, type of iron oxide, and composition of gas on the gas and solids conversions during reduction and oxidation. A baffled free-fall solids system was also found operable. The short residence time of about 5 seconds limited conversion of the solids.

Jan 1, 1961

By J. B. Gayle

Numerous investigators have studied the addition of inert4 substances to coking blends. Generally, the results have yielded trends applicable only to the particular coals and inerts studied. Recently, somewhat more general results were obtained for cokes produced from blends containing added inerts, using the sole-heated oven. The present investigation represents an extension of this work to include a wider range of inerts and to determine the applicability of the various conclusions to cokes produced with the Tuscaloosa oven. The results indicated that an increase in dry-coal charge density of 1 pound per cubic foot (p.c.f.) caused a corresponding change in the hardness (1/4-inch tumbler index) of Tuscaloosa oven cokes of 0.9 percentage points. This value compares favorably with the value of 0.7 determined previously for the sole-heated oven and Bureau of Mines-American Gas Association (BM-AGA) retort.

Jan 1, 1961

By W. P. Haynes

The Bureau of Mines has been studying a modified steam-iron process using coal-derived producer gas for making either hydrogen plus carbon monoxide or methane. To provide a guide for this experimental study, compositions of equilibrium product gases for the reaction of steam plus carbon dioxide with iron were calculated and are discussed in this report. The calculations, which are described in this report, are based on thermodynamic data in the literature and cover temperatures from 800° to 1,300° K., pressures from 1 to 30 atmospheres, and hydrogen-to-carbon atomic ratios in the gas of 4 to 12. The equilibrium gas compositions are discussed in regard to making hydro-gen, carbon monoxide, and methane in the oxidation step of the modified steam-iron process. From the viewpoint of thermodynamics alone, assuming the reactions reach equilibrium, the discussion considers the effects of temperature, pressure, and composition of feed gas upon the composition of the product gas, the degree of oxidation of the iron, and the possible deposition of carbon. The results indicated the following: (1) Nearly all the carbon can be converted to methane at low temperatures (800° to 900° K.) and high pressures (over 20 atmospheres); (2) to obtain high yields of synthesis gas, high temperatures are required. For example, at 30 atmospheres, a temperature over 1,200° K. is required to convert 60 percent of the steam plus carbon dioxide to hydrogen plus carbon monoxide. Lower temperatures may be used at lower pressures) (3) oxidation of the iron increases with increasing pressure and decreases with increasing temperature; and (4) process conditions favoring carbon deposition were found within the range of variables studied, but it is thermodynamically possible to operate the oxidation process with steam and carbon dioxide outside this range of carbon deposition.

Jan 1, 1961

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By J. J. Wallace

This report describes the initial phase of Bureau of Mines research in the hydraulic mining of bituminous coal. The mining site and equipment are described, and the test procedures and results obtained with a bar-mounted monitor are given. Tests showed that hard Pittsburgh-bed coal can be mined hydraulically from a solid face at water pressures of 4,000 pounds per square inch.4 Coal was penetrated to a depth of 4 feet in 20 seconds with 225 gallons of water per minute coming from a 3/8-inch nozzle at 4,000 pounds per square inch pressure. Some difficulty was encountered in cutting the binders occurring in the coal; it was not possible Lu penetrate directly the overlying draw slate.

Jan 1, 1961

By S. R. Borrowman

This investigation by the Bureau of Mines was undertaken to develop information on the extractive metallurgy of thorite ores because potential ore bodies of this mineral have been found recently in Colorado, Idaho, and Montana. Basic information on thorite ore treatment that would be useful in appraising the potential of these and other domestic thorium resources was developed. The work was done mainly on thorite ore containing 3.87 percent ThO2 from the Powderhorn district, Colo., and on a composite sample containing 0.52 percent ThO2 from the Wet Mountains district, Colo. Limited tests of d corroborative nature subsequently were made on a sample containing 2.30 percent ThO2 from the Lemhi Pass area on the Idaho-Montana border.

Jan 1, 1962

By S. R. Borrowman

Physical beneficiation, leaching, and solvent extraction investigations were made to recover a high-grade thorium oxide product from Bald Mountain, Wyo., conglomerate. The monazite in the Bald Mountain deposit contains 8.8 percent Th02 and, therefore, is higher in thorium content than the usual domestic or foreign monazite. A sample of composited drill cuttings for the study contained 4.3 pounds of monazite per ton of are. The work showed that the monazite, although unusually fine grained and friable, could be concentrated by tabling and magnetic treatment to yield a product assaying 5.65 percent Th02 with a recovery of 61 percent of the thorium. Subsequent decomposition of the concentrate by treatment with sulfuric acid and solvent extraction of the resultant solution with a primary aliphatic amine yielded a thorium oxide product of 99-percent grade.

Jan 1, 1962

By Willard L. Hunter

The separation of tantalum and columbium by solvent extraction was under-taken as part of the Bureau of Mines research program to improve methods for extracting, separating, and reducing these elements to metal. The diethyl ketone aqueous HCl-HF system was one of several systems studied to determine the effect of metal and acid concentrations in aqueous solutions upon the transfer of tantalum and columbium into selected ketones. The tantalum-columbium oxide mixture used in this investigation was obtained by chemical extraction from Geomines slag. The investigation showed that tantalum 99.4 percent pure and columbium 97.2 percent pure can be produced by the selective transfer of tantalum into diethyl ketone from a solution of 2-N HF and 1-N HC1. The relatively low acid concentration necessary for tantalum transfer and the excellent selectivity of the system recommend its use for the separation of tantalum and columbium.

Jan 1, 1961

By A. W. Henderson

The growing importance of halide metallurgy for preparing high-purity metals has stimulated research to extend halogenation reactions to the direct extraction of metals from low-grade sources. This Bureau of Mines investigation involves a pioneering study of chlorination reactions in the presence of a fluorine donor. Tin slags containing tantalum and columbium and a zircon concentrate containing a relatively high ratio of hafnium to zirconium were studied. Direct chlorination of these materials at 500° C. yields only a 5-percent conversion of tantalum and columbium or zirconium and hafnium to anhydrous chlorides. This investigation showed that small additions of calcium fluoride to the reaction increased the recovery of tantalum and columbium to 95 percent and the recovery of zirconium and hafnium to 27 percent. These results were achieved with ratios of calcium fluoride to mineral or slag of only 0.2. Silica, the major impurity in the materials studied, was found to be converted to silicon tetrafluoride during chlorination in direct proportion to the quantity calcium fluoride added to the charge. However, large additions of calcium fluoride decreased the volatility of the resulting halides of tantalum, zirconium, and hafnium. Smaller amounts of calcium fluoride also favored recovering minor metal constituents in the zircon concentrate (uranium, thorium, and rare earths).

Jan 1, 1962

By L. M. Burman

The phase-boundary pressure required to maintain a natural hydrocarbon fluid in a single phase must be considered in planning the recovery of reservoir liquids by miscible-phase processes. The change in the phase-boundary pressure at reservoir temperature that results when a light component or a mixture of light components is added to a reservoir fluid is an especially important consideration. The cricondenbar pressure (maximum phase-boundary pressure) and the critical pressure are unique correlated pressures that have been utilized to calculate the change in phase-boundary pressure that may result when the composition of a reservoir liquid is altered by an additive. In this study one reservoir oil and three gas-condensate fluids are used as examples. Correlations pertaining to the critical and cricondenbar states in chapters 4 and 5 of Bureau of Mines Monograph 10 (3)5 were used to demonstrate how butane and lighter components added to these reservoir fluids affect their phase-boundary pressures.

Jan 1, 1962

By R. V. Higgins

Many contributions to methods of forecasting the performance of waterfloods of a five-spot pattern have been made by investigators. In most of these forecasting methods, a previously selected sweep efficiency is used, and other simplifying assumptions are employed to obtain the objective. In this paper the calculated oil recoveries from several five-spot single- and multiple-layer stratified reservoirs were made with a minimum of assumptions, and because of the techniques used, no previously selected sweep efficiency was required. As a result, the accuracy of the forecast is increased. Permeability curves and continuously changing saturation gradients are used in every section of the pattern. By means of a potentiometric model, the flood pattern is divided into channels, the centers of which are the streamlines. The channels are divided into cells. As flood water enters, the permeability and saturation of each cell change with time. In this study the production from multiple-sand layers of different absolute permeability but with the same relative permeability-saturation relations are combined. The results are shown for a single- and 10-layer reservoir with a permeability variation of 0.60. The oil rate, water-oil ratio, and recovery are shown as functions of time for a 2- and 20-centipoise oil starting in primary phase and after fill-up.

Jan 1, 1962

By Wesley Holmes

Concentrating, nodulizing, and smelting studies were conducted at the Albany Metallurgy Research Center of the Bureau of Mines to determine whether (1) western iron ores of the type found in the Carter Greek deposit near Dillon, Mont., could be utilized; (2) concentrates of acceptable grade with good iron recovery could be attained by wet-magnetic beneficiation; (3) nodulized concentrates could be smelted with reductants readily available in Montana; (4) iron concentrates could be smelted without prior agglomeration; and (5) high-purity iron could be produced directly from high-grade concentrates, Three small samples and two tonnage samples from the Carter Creek deposit were uniform in chemical composition, and their iron content averaged about 31 percent. They were found to be banded gneisses, and magnetite was the principal iron-bearing mineral.

Jan 1, 1962