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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 Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation.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 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 R. W. Stahl

Increasing use of continuous miners, especially the boring type, has focused attention on the inadequacy of face ventilation in coal mines. The bulk of the machine, the rapid advance of working faces, and the increased liberation of methane from the larger expanse of freshly exposed coal surfaces have created ventilation problems that were unknown with conventional mining equipment. Ignition of gas, especially that caused by machine bits striking hard rock or pyritic inclusions, have increased at an alarming rate. As the mines penetrate beds under thicker cover at an ever-increasing rate of face advance, this problem will probably increase unless face ventilation is improved. A previous survey, described in Bureau of Mines Report of Investigations 5414, Auxiliary Ventilation of Continuous Miner Places, disclosed that auxiliary fans with tubing generally improved circulation of air and removal of gas at the face. The study here reported attempts to examine, face ventilation at various mines and to note any plan or innovation of. air coursing that industry might adopt to reduce the danger of gas ignition. ACKNOWLEDGMENT The mines visited were very cooperative in the study-and-generously supplied any data requested.

Jan 1, 1960

By E. D. Wilson

This is the second of a series of progress reports describing work undertaken at the San Manuel copper mine to study the geologic factors influencing block caving of the deposit. The first report described the work done from April 1954 to March 1956.3/ This report describes the progress from March 1956 through March 1958 and presents additional maps, factural data, inferences, and conclusions resulting from a continuation of the underground geological work. As outlined in these reports, the study thus far has shown that the principal geologic factors affecting block caving are structure, rock types, alteration, mineralization, oxidation, and presence of water. Structure is fundamentally the most important. Systematic fracturing governed the extent and grade of primary ore mineralization and tangibly affects the subsidence or ground movement, which extends from the mine workings to the surface because of the block caving.

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 H. E. Powell

The mineral dressing research here reported is part of a continuing program by the Bureau of Mines to develop new or improved concentration processes for oxidized or partly oxidized lead and zinc ores. A sample of low-grade sulfide-oxide, lead-zinc ore from Jasper County, Mo., containing galena, cerussite, pyromorphite, hemimorphite, smithsonite, and sphalerite was concentrated by froth flotation and tabling to a grade of 66 percent lead. Because of the presence of a high content of slime-size values, the overall recovery of lead was limited to 64 percent at this grade. Tests to recover the zinc by froth flotation and by gravity concentration did not give satisfactory results. INTRODUCTION Since its establishment, the Rolla Metallurgy Research Center has con-ducted studies of base metals as a part of its overall program (1, 2, 3, 4, 5,6,7).3/ This research has been, and is, directed to beneficiating complex and submarginal ores, to retreating rejects from commercial installations, and to developing fundamental data.

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. L. Montgomery

Electronegativities of the rare-earth elements were calculated from heats of formation. The values obtained from different compounds varied widely. The postulates of Pauling's electronegativity theory were interpreted for bonds that are primarily ionic; the study showed that many compounds obey rules of the form expected. Revised electronegativity values are given for the more electropositive elements, including the rare-earth metals (which are near magnesium in electronegativity). Estimates of un-known heats of formation are made from electronegativities and are compared with other estimates. INTRODUCTION Calculation of the electronegativities of the rare-earth elements is interesting to show how these metals stand relative to the other metals and to each other, and also possibly to systematize the thermochemical data on them.

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 D. E. Ingersoll

This report describes the preparation characteristics of anthracite from the Mammoth and Holmes veins in Schuylkill County, Pa., as determined by the Federal Bureau of Mines laboratory separations at specific gravities of 1.50 to 1.90. The Holmes vein anthracite contains approximately 13 percent ash, and the Mammoth vein contains about 9 percent as fed to the breaker. Crushing Broken, Egg, and Stove sizes from each vein produces Pea-size anthracite of lower ash content than that contained in Buckwheat No.1 size and smaller. The Buck-wheat No.5 size has the highest ash content of all the sizes examined. Potential recovery from a mixture of the two veins as received at the breaker, separated at 1.90 specific gravity, is approximately 64 percent of the feed at 11.0 percent ash. The same materials separated at 1.80 specific gravity yield about 61 percent with an ash content of 10.1 percent. All rejects are from the Holmes vein, because the entire Mammoth material is less than 10.0 percent ash.

Jan 1, 1960

By D. J. Bauer

Liquid-liquid extraction techniques were investigated by the Federal Bureau of Mines for the fractionation of rare-earth solutions. Separatory funnel work using tri-n-butyl phosphate (TBP) for extracting ceric nitrate from solutions containing sulfate ion resulted in almost complete extraction. Similar tests using primary amines for splitting trivalent rare-earth pairs and fractions gave promising results. The ceric nitrate extraction procedure was scaled-up by use of pressure-bubbler equipment, a series of spray towers for extraction, washing, and stripping. In this case only 84 percent ceric nitrate extraction efficiency was achieved. This work was done using dilute sulfuric acid for stripping.

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

By W. L. Hunter

This report describes results of beneficiation and smelting studies conducted by the Federal Bureau of Mines on chromite samples from the Emma Belle and Seiad Creek prospects in the Seiad Creek area, northern California. Samples were chosen from this area because the ore is typical of disseminated types that represent a sizable domestic reserve. The two samples were similar in composition, and both responded in like manner to gravity beneficiation. As the ore was banded, considerable coarse gangue was rejected in laboratory sink-float from a minus-3/4-inch, plus-6-mesh fraction without excessive chromium loss at a medium density of 3.32. An average of 85.6 percent of the chromium was recovered in the sink product, which analyzed 35 percent chromic oxide (Cr203). Tabling yielded concentrates containing 49 percent or more Cr203; however, recoveries, ranged from only 33 to 45 percent. A combination of tabling and electrostatic separation of the table middlings showed that the chromium recovery could be increased to about 73 percent; the composite concentrate averaged 53 percent Cr203.

Jan 1, 1960