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By Raymond O. Dannenberg

The gas-combustion retort developed by the Federal Bureau of Mines at the Rifle Oil Shale Project near Rifle, Colo., is a continuous, gravity-feed retort. The heat required to convert the kerogen in the oil shale to liquid oil is generated by the combustion of product gas and carbonaceous residue remaining on the retorted shale after the kerogen has been converted to oil, gas, and residue. A study of the effects of the process variables on retort operation, product yields, and product properties is important to the successful solution of the problems encountered in the development of a satisfactory process. Statistical methods were used to design the experiments and analyze the effects of the rate of shale throughput, the composition of dilution gas, the height of the shale bed above the air entry, air-gas distributor design, shale size range, and the ratios of the flow rates of the various gas streams entering the retort to the rate of shale throughput.

Jan 1, 1960

By F. P. Haver

The purpose of this investigation was to determine the effect of common impurities, that is, oxygen, nitrogen, carbon, and iron, on the Brinell hardness of electrolytic titanium. On a weight basis, nitrogen had the greatest hardening effect, followed by oxygen, carbon, and iron in order. The hardening effects of oxygen and carbon were almost identical up to a concentration of approximately 0.1 percent by weight. Above this concentration, the relative hardening effect of carbon decreased rapidly, possibly because of its limited solid solubility in a-titanium. Hardness vs. composition curves for both oxygen and nitrogen were essentially straight lines over the range of Brinell hardness numbers (B.h.n.) covered in the investigation. The hardness of titanium was also determined as a function of the percentage of impurity atoms. On this basis, iron in concentrations up to 0.17 atomic percent had a greater hardening effect than either oxygen or carbon. INTRODUCTION Determination of the as-cast hardness of arc-melted titanium is a method of quality control widely used in industry. Numerous studies4/ have been made of the effect of impurities on the hardness obtained by this method. However, most of them have been based on the use of either iodide titanium or commercially pure Kroll sponge (B.h.n. >90), as a starting material.

Jan 1, 1959

By E. Morrice

The metallurgical laboratory data developed in this study indicate an improved electrowinning process for producing higher purity cerium ingot. A typical sample of the Reno electrocerium contains 99.9 weight-percent cerium and the following impurities: Total other rare-earth elements, less than 0.04 percent; iron not detected; silicon and aluminum, less than 0.02 percent each; calcium plus magnesium, less than 0.01 percent; carbon, 0.01 percent; oxygen, 0.002 percent; hydrogen, 0.0003 percent; and nitrogen, 0.0015 percent.

Jan 1, 1960

By D. W. Frommer

Mineral dressing research was conducted by the Federal Bureau of Mines under a cooperative agreement with the St. Joseph Lead Co., on three samples of iron ore from the Pea Ridge deposit in central Missouri. The objective was to provide information on how to upgrade these submarginal ores and produce marketable concentrates. Samples were prepared from drill-hole cores of similar composition and character to produce (1) a medium-grade mixed hematite and magnetite, (2) a high-grade mixed hematite and magnetite, and (3) a high-grade magnetite. In all three ores phosphorus and sulfur constituted objectionable impurities; excessive amounts of silica were also present in the medium-grade ore.

Jan 1, 1960

By Charles W. Huggins

DEVELOPMENT of the electron microscope has permitted man to examine many small objects that could not be resolved by the light micro-scope. Diffraction, spherical aberration, and chromatic aberration are the main factors that limit resolution to about two-tenths micron with the light microscope. No matter how perfectly a light microscope is constructed and operated, it cannot possibly resolve points separated by less than two-tenths micron. Rapid development following World War II has produced many electron microscopes capable of 20 A resolution. Fibrous inorganic minerals are well suited for electron microscopic study. Many micrographs of chrysotile have been published, but electron microscopic study of the amphiboles has been somewhat neglected. New techniques in sample preparation have simplified the study of fibrous material. Ultrasonic energy has been very helpful in sample dispersion. This publication contains a representative group of electron micrographs of natural inorganic fibers that have industrial value. These fibers commonly are referred to as the asbestiform minerals. The Bureau hopes that the knowledge gained through electron microscopy and other scientific study of the natural inorganic crystalline fibers eventually will lead to the production of synthetic fibers that will satisfy the requirements of industry.

Jan 1, 1959

By Eldon C. Pattee

THE BUREAU OF MINES began an investigation of tungsten resources of Montana in September 1953. This report presents information obtained from July 1955 to September 1957 on tungsten deposits in and near the Mount Torrey batholith. The batholith comprises part of the Pioneer Mountains of Beaverhead County in the southwest corner of Montana. Included in the report are assays and preliminary-examination data on 22 properties. Tungsten minerals are known to occur in 19 of the properties. The major producer is the Brown's Lake mine which has produced more than 625,000 tons of ore. Nearly all of the deposits are in the Lost Creek, Utopia, and Bald Mountain mining districts along the east and south margins of the Pioneer Mountains. The districts are less than 27 miles from Dillon, Mont.

Jan 1, 1960

By Joel N. Van Sant

THIS REPORT describes the occurrence, mining, and use of refractory clay in Colorado within Region III of the Federal Bureau of Mines, which includes the States of North arid South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona. Field work by the Bureau of Mines, United States Department of the Interior, included examination of active and abandoned refractory-clay mines as well as a reconnaissance survey and sampling of numerous clay-bearing formations exposed in Colorado. Information from the survey and the sampling will help guide private industry in its search for virgin sources of refractory clay. Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation. Most of the refractory clay mined in the Denver-Golden district of Colorado is not used for refractory purposes but is blended with other clays in the manufacture of structural clay products. The predominantly flint-clay de-posits in the Pueblo and Fremont County districts are mined and utilized chiefly in fabricating refractory products.

Jan 1, 1959

By J. B. Zadra

Tungsten metal, chemically equivalent to commercial grade, is produced by electrolysis of impure tungsten compounds or scheelite in an alkali, phosphate or borate electrolyte. A preliminary investigation of fused-bath electrolysis shows the effect of electrolyte composition, temperature, and current density on current efficiency, yield, crystal structure, and purity of product. Experiments show that tungsten can be electrowon from scheelite in a fused alkali, phosphate, or borate bath with similar results. Studies on electrolyte composition show that the addition of sodium chloride is essential to both electrolytes in treating scheelite. Although its main function is to react with or flux the CaO, it also increases the bath fluidity. Temperature studies revealed optimum ranges between 900° and 1,100° C.; 900° C. proved satisfactory for tungsten trioxide, and 950° to 1,050° C. for scheelite. Current efficiencies were satisfactory for all current densities ranging from 10 to 57 a./dm.2. Yields were 400 to 650 g./kw.-hr. over the same current-density range. Crystal size and purity of the product are functions of temperature, current density, and amount of impurities in the electrolyte. Deposited crystals vary in shape from spherical grains to clusters of dendritic hexagonal needles, and in size from smaller than 35 to 570 microns. The purity of the tungsten metal produced ranges from 99.7 to 99.94 percent.

Jan 1, 1959

By E. D. Calvert

Molybdenum has been successfully cast into static and rotating molds in conventional equipment used for casting titanium and zirconium. Melting was accomplished by using an arc potential of 36 to 40 volts with a current of 10,000 amperes. Pouring efficiency, after a skull had been formed in the crucible, averaged 70 percent. Techniques are described by which four successful castings were made. Tensile properties on specimens cut from one centrifugally cast tube averaged: Tensile strength, 39,800 p.s.i.; yield strength (0.1 pct. offset), 35,300 p.s.i.; elongation, nil; reduction in area, nil; impact strength, 2 ft.-lb.; hardness DPH (diamond pyramid hardness) 180. Mold reaction was not evident in shapes cast in machined graphite. This was not true, however, for rammed graphitic-base molds.

Jan 1, 1960

By R. F. Tenney

This report has been prepared because little detailed information has been published on the production and use of anthracite producer gas for industrial-process and brick-kiln heating. To obtain this information, an investigation was conducted by the Federal Bureau of Mines in cooperation with a building-brick manufacturer (firing both periodic and tunnel kilns with anthracite producer gas) and with a manufacturer of anthracite-gas producers. In addition to a study of available plant records, 2 weeks was spent in systematic observation and measurement during regular operation of the Hazleton Brick Co. plant, Hazleton, Pa., in July 1953. This report presents the results of this investigation and a description of producer and periodic-kiln equipment, operating procedures, and labor requirements. A summary of the conditions of producer and kiln operation is given for the 2-week observation and for the 11 preceding months. The two 10-foot standard anthracite-gas producers consumed 301 tons of Rice and Buckwheat No. 1 anthracite, as delivered, averaging over 13,000 B.t.u. per dry pound during the 2-week period, with a producer hot-gas efficiency of 95 percent, at an average gas offtake temperature of 5400 F. The yield of gas5/ of 153 gross B.t.u. per cubic foot amounted to 140,000 cubic feet per ton of fuel as fired, or 73,500 cubic feet per kiln heating hour, which was sufficient for kiln requirements.

Jan 1, 1960

By Robert L. Rough

This report presents the results of an investigation by Federal Bureau of Mines engineers of water-injection projects in the northwestern Pennsylvania and southwestern New York area, where oil-producing wells have been converted from pumping to flowing. Data from 24 leases converted to flowing were collected and examined. Only 10 leases had information of significant scope for inclusion in the final analysis. The projects were classified in one of two categories. Group I consisted of leases operated to permit an evaluation of operational changes in terms of existing pressure differentials between injection and producing wells. Group II included remaining properties, for which enough information was available to justify an economic analysis but which did not have sufficient production data to support an engineering study because of radical changes in operational techniques. Variations in production and costs resulting from conversion to flowing were examined for production methods, well-spacing and completion techniques, and reservoir characteristics. Where water-injection rates were constant, oil production usually decreased rapidly at the time of conversion; production then increased slightly for 6 to 8 months before resuming a normal decline rate considerably below the estimated pumping rate. The abrupt decrease in production after conversion is indicative of lower pressure differentials between injection and producing wells, caused by the increased hydrostatic head in the producing wells.

Jan 1, 1960

By G. R. Strimbeck

The Federal Bureau of Mines has been developing processes for producing synthesis gas directly from coal, oxygen, and superheated steam. An atmospheric-pressure pilot plant was constructed and operated to: 1. Determine the operability of the plant for gasifying coals of different ranks under various operating conditions. Listed in decreasing order of rank, these coals included a Pennsylvania anthracite, a bituminous A coal from the Sewickley bed, West Virginia, and a subbituminous C coal mined in the Lake de Smet region of Wyoming. 2. Determine the effect of varying operating conditions on: (a) Standard cubic feet (std.c.f.) of oxygen and pounds of coal of different rank required to make M std.c.f. of product gas (carbon monoxide plus hydrogen); (b) carbon gasified, percent; (c) exit-gas temperature, degrees F.; and (d) heat loss, B.t.u. per pound coal. 3. Compare the gasification characteristics, indicated in item 2, of coals of different rank: Bituminous A, anthracite, and subbiturninous C. 4. Determine the concentration of dust in the gases produced and the efficiency of dust removal, and investigate the relation between the sulfur content in the coals gasified and the gases produced.

Jan 1, 1960

By Arthur Matzick

The oil shale from the Mahogany zone of the Green River formation in northwestern Colorado has the greatest potential in the United States for early utilization. A large reserve of adequately rich shale is available to support a sizable industry, and crushing of tremendous tonnages will be required if conventional processing methods are used. This report presents Bureau of Mines data on crushing experiments, physical properties, and related information for Colorado oil shale. Among the properties important to crushing are slab-forming tendency, resilience, slippery character of the richer grades, and heterogeneous nature of an average charge of Colorado oil shale.

Jan 1, 1960

By A. U. Christensen

THERMODYNAMIC data for many of the common interoxidic compounds are seriously lacking, and appraisal of possible ceramic or metallurgical applications depends upon dubious estimates. In particular, high-temperature heat-content estimates may be invalid because of unknown phase-transformations. This paper reports experimental heat-content values above 298.15° K. for five interoxidic compounds-the aluminates of lithium and sodium (LiAlO2 and NaAlO2), the ferrites of lithium and sodium (LiFeO2 and NaFeO2), and lithium titanate (Li2TiO3), as obtained by the Bureau of Mines. Sodium aluminate, sodium ferrite, and lithium titanate were found to have previously unknown transformations in the crystalline state. The heats and temperatures of these transformations were evaluated as were also the heats and temperatures of fusion of sodium ferrite and lithium titanate. The heat-content results are assembled in both tabular and algebraic-equation form for use in conducting thermodynamic calculations at temperatures in the range 298°-2,000° K.

Jan 1, 1960

By R. V. Higgins

As part of a study of application of the Buckley-Leverett method to an analysis of oil-reservoir performance covering a wide range of relative permeabilities and oil saturations, a method has been devised for quickly deter-mining average water saturation at breakthrough from relative permeability data. The base for the relative permeability used in the report is either the permeability to air or the effective permeability to oil at the irreducible water saturation. The permeability to air also was used because of the large backlog of air permeabilities available to reservoir engineers. The basic data were calculated by an electronic computer and are presented in a single graph from which the point of breakthrough may be obtained. In this study the water saturation at the beginning of the depletion is the connate or interstitial or irreducible water saturation. These water saturations are considered to be synonymous and to have a practical value.

Jan 1, 1960

By E. G. King

THIRD-LAW entropy data for zirconium-containing compounds are sparse. Kelley a lists entropies at 298° K. for the oxide, tetrachloride, nitride, and silicate, as well as for the metal. The present paper presents heat capacities between 51° and 298° K. and entropies at 298.15° K. for the zirconates of the alkaline-earth metals-calcium, strontium, and barium. The authors believe magnesium zirconate does not exist as a stable compound at room temperature. Entropies of formation from the constituent oxides also are given. MATERIALS The materials used in this investigation were synthesized and analyzed in the Berkeley Laboratory of the Bureau of Mines. Calcium zirconate was prepared by heating an intimate mixture of reagent-grade calcium carbonate and pure zirconia for 30 hours between 1,200° and 1,300° C. and for 32 hours between 1,400° and 1,500° C. As part of the heating schedule, the sample was ground and mixed seven times. Periodic analyses and minor adjustments of composition were made. Analysis of the final product gave 31.19 percent calcium oxide (theoretically 31.28 percent) and 68.67 percent zirconia (theoretically 68.72 percent). The X-ray diffraction pattern agreed with that in the ASTM catalog.

Jan 1, 1960

By T. E. Gray

This report describes the preparation characteristics of the more significant coalbeds in Monongalia County, W. Va. It is one of a Bureau of Mines series planned to determine coals suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.5 million tons of coal was produced in Monongalia County in 1957, of which more than 7 million tons was cleaned mechanically in 8 cleaning plants. On January I, 1954 the Bureau of Mines estimated that 1,576 million tons of recoverable coal remained in the county in beds 28 inches or more thick.

Jan 1, 1960

By J. H. Holden

The Federal Bureau of Mines is doing research and development work on a pressure-gasification pilot plant for producing synthesis gas directly from pulverized coal, oxygen, and steam. A pressure-gasification pilot plant has been constructed, and an investigation was made with the following basic objectives: 1. Determining the effect of varying pressure (75, 100, 150, and 300 p.s.i.g.), coal rate (400, 700, and 1,000 pounds per hour), and oxygen-to-coal ratio (8 to 11 std, c,f. per pound), on percentage of carbon gasified, oxygen and coal requirements per unit of CO + H2 produced, exit-gas temperature, and heat loss. The steam-to-coal ratio was maintained at approximately 0.3 pound per pound. 2. Development of a stabilized gasification zone or reaction space. 3. Improvement in operability of the pilot plant.

Jan 1, 1960

By C. M. Frost

Two Federal Bureau of Mines recycle hydrogenation experiments to prepare catalytic cracking feed stock were made at 3,000 pounds pressure with crude shale oil retorted from Green River (Colo.) shale in the gas-combustion retort. The hydrogenated product from the first experiment, made at 784° F., was used for investigating the effects of nitrogen content on catalytic cracking yields and for determining the quality of the catalytically cracked gasoline. Hydrogenated product containing 0.14 percent or more of nitrogen produced less gasoline when cracked in a CAT "A" unit than was obtained from East Texas light gas oil cracked at the same conditions; product containing 0.10 percent or less nitrogen produced a quantity of cracked gasoline equal to that obtained from the East Texas light gas oil. The catalytically cracked gasoline had research octane numbers calculated to be approximately 95 clear and 103 with 3 ml. of tetraethyl lead. The principal product from the second experiment, made at 828° F., was a low nitrogen content gas oil which was used for investigating the yields of cracked products obtained when it was catalytically cracked to different degrees of conversion. Yields of cracked products, when plotted as functions of conversion, were essentially the same, within the experimental range of the data, as published yields from catalytic cracking of East Texas heavy gas oil; however, yields from cracking the shale-oil product did not display the sensitivity to change of cracking temperature that has been found for East Texas gas oil.

Jan 1, 1960

By Oliver C. Fursman

This work was conducted to determine the feasibility of producing aluminum-silicon alloys in a pit-type, three-phase electric-arc furnace. Two carbon-lined furnaces were used in the tests. The power input ranged from 120 to 240 kw. in the small furnace and from 420 to 460 kw. in the large furnace. Energy consumption ranged from 5.3 to 11.5 kw.-hr. per pound of alloy produced and electrode consumption, from 240 to 510 pounds per ton of alloy produced. A wide range of crude aluminum-silicon alloys was produced by direct smelting of clays or similar aluminum silicate raw materials, using hogged fuel or wood chips as the major source of carbon in the furnace charge, and silicon of high grade was produced by smelting quartz. The aluminum content of the aluminum-silicon alloys ranged from 15 to 55 percent. Alloys produced from a white opaline-silicate clay were relatively free of iron, titanium, and other impurities. Those produced from western fire clays and kyanite, although richer in aluminum, contained considerable amounts of impurities. The purity of the alloys depended largely on the composition of the raw materials.

Jan 1, 1960