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By P. G. Pigott

The lack of technical information regarding the physical characteristics of kaolins and bauxitic kaolins, rejected during the mining of bauxite near Eufaula, Ala., has retarded their commercial utilization. This investigation was undertaken to determine their behavior when used in refractories. Ores were evaluated as refractory raw materials by compounding dry-press mixtures and specialties following procedures common to the industry. Products now on the market were used for comparison in laboratory evaluation.

Jan 1, 1959

By O. Q. Leone

Excellent metal quality, with lower power requirement, is attained in electrorefining titanium by using internal heating of the fused-salt bath. An internal heater provides more effective heat utilization, simplifies structural components in cell design, and prolongs cell life by eliminating direct application of heat to the cell container. This Bureau of Mines report covers one phase of the research in progress at the Electrometallurgical Experiment Station at Boulder City, Nev., for improving the techniques and lowering the total power requirement for electro-refining titanium metal.

Jan 1, 1959

By R. B. Fisher

This report gives the results of mineralogical research on the Nicaro (Cuba) nickel ores and plant products. These studies were made under a cooperative agreement with the General Services Administration (GSA) of the U. S. Government. The purpose of the investigation was to obtain fundamental data that would be useful to other GSA contractors concerned with the Nicaro ores in their research on reduction roasting, leaching, and other phases of the project; and to the metallurgical staff of the Nicaro plant in Cuba. The overall objective of the combined research was to provide data to accomplish metallurgical improvement in the operations of the U.S. Government-owned plant at Nicaro, Oriente Province, Cuba. Particular emphasis is placed on improving the recovery of nickel from the ores and on the possibility of recovering other valuable constituents, especially cobalt. This study presents the physical and chemical characteristics, mineral associations, differential thermal analyses in controlled atmospheres, and X-ray studies of the ores and plant products. The nickel ores, serpentine and laterite, were from the Ramona-Lama Mulo and Ramona ore deposits. Serpentine ore consisted of serpentine-group minerals, basic iron oxide, magnetic iron oxides, chromite, olivine, enstatite, anthophyllite, cryptocrystalline quartz, wad, and a trace of calcite. This ore contained 1.6 percent nickel, 0.05 percent cobalt, 0.86 percent chromium, and 17.4 percent iron. Laterite are was composed principally of goethite with some altered serpentine, quartz, chromite, wad, magnetite, maghemite, and hematite. It carried 1.3 percent nickel, 0.11 percent cobalt, 1.9 percent chromium, and 48.4 percent iron.

Jan 1, 1959

By William J. Campbell

This report describes a Bureau of Mines study undertaken to determine the applications and limitations of solution techniques as a general method of fluorescent X-ray spectrographic analysis. Systematic errors due to variations in particle size, surface preparation, and sample inhomogeneity are eliminated by the use of solutions. The range of applicability of fluorescent X-ray spectrography is increased in two ways: (1) Samples in the form of wire, filings, turnings, etc., can be analyzed as solutions, and (2) samples submitted as solutions can be analyzed as received 0 The lower limit of detectability varies from 0.14 gram per liter for sulfur, atomic number 16, to 0.0015 gram per liter for strontium, atomic number 38. Most elements have limits of detectability between 0.02 and 0.002 gram per liter.

Jan 1, 1959

By William A. Stickney

The zirconium-hafnium separation plant at Albany, Oreg., was the result of a chain of events that started with studies by A. R. Kaufmann at the Massachusetts Institute of Technology. Variations in the listed neutron-absorption cross-section of zirconium caused him to suspect a misprint. As a result of these discrepancies and following his suggestions, Oak Ridge scientists made studies establishing a value of 0.4 barn or lower. This meant that the potential of zirconium for reactor application was greatly enhanced. Since hafnium is invariably associated with zirconium and has a high neutron cross-section, it was necessary that an efficient hafnium-separation method be developed before the superiority of zirconium as a structural material in nuclear reactors could be realized. The Albany plant was built and operated for the Atomic Energy Commission (AEC) under Letter Agreement AT-(11-1) -140, patterned after a plant operated by the Carbide and Carbon Chemicals Corp. at Oak Ridge, Tenn. Construction was begun in April 1951. Hafnium was to be extracted preferentially as hafnium thiocyanate from an aqueous mixture of zirconyl and hafnyl chlorides in hexone (methyl isobutyl ketone) by a liquid-liquid countercurrent system.

Jan 1, 1959

By V. B. Dale

This is one of a series of reports covering the mineral resources of the Nation. It describes briefly most of the known tungsten deposits in Yuma, Maricopa, Pinal, and Graham Counties, Ariz. Most of those described were examined by the author. An effort was made to determine the position of the various deposits by section, township, and range and to give accurate road direction to each property from a prominent landmark. All available maps have been used in making these determinations, but in unsurveyed areas it was necessary to make approximate projections of subdivisions. The township and range numbers refer to the Gila and Salt River base and meridian.

Jan 1, 1959

By V. B. Dale

This paper is one of a series covering the mineral resources of the Nation. It briefly describes most of the known tungsten deposits of New Mexico. Most of the descriptions are from field examinations by the senior author. Reported tungsten occurrences that were not visited are listed below: Colfax County: Occurrences of ferberite in thin veins in Willow Creek near Elizabethtown.4/ Dona Ana County: Small, low-grade occurrences of scheelite near the summit of the Organ Mountains about 15 miles east of Las Cruces. Hidalgo County: Scheelite reported in the Daisy mine 7 miles southeast of Hachita. Ores are carbonates containing copper, gold, silver, and bismuth.5/

Jan 1, 1959

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 J. D. Ramsdell

To obtain information on the effects of cobalt on microstructure and tensile properties of titanium-vanadium-cobalt alloys, the composition ranges of 4 to 16 percent vanadium with 1 to 4 percent cobalt have been studied. The beta phase was not completely retained with vanadium additions up to 16 weight-percent or in the same alloys containing up to 4 percent cobalt.

Jan 1, 1960

By Walter W. Fowkes

Leonardite is a coallike substance, similar in structure and composition to lignitic coal and believed to be derived from lignitic coal by the process of natural oxidation. Leonardite is little known outside lignite-producing areas and has been developed commercially only to a minor extent. The higher oxygen content and less compact structure of leonardite, compared with lignite, make it undesirable as a fuel but indicate that it has potential as a source of chemicals and for other nonfuel uses. It is a convenient source of humic acids. The United States has a large natural reserve of leonardite; furthermore, it can be produced in the laboratory under controlled conditions. The significant elemental difference between leonardite and lignite is the oxygen content (leonardite, 28-29 percent; lignite, 19-20 percent). The higher oxygen content of leonardite is due entirely to a Larger number of carboxylic acid groups. This fact explains the 17-Cold increase in alkali solubility of leonardite. Spectral studies indicate that the material is mixed salts of humic acids.

Jan 1, 1960

By L. J. Kane

Conventional methods for determining the size of dust suspended in a gas require that agglomerates (clusters of particles) first be broken into particles, but in evaluating industrial dust-removing equipment the size of the agglomerates as they actually exist in the gas stream is far more important. This paper presents results of an investigation by the Federal Bureau of Mines to develop methods for determining the size of dust agglomerates suspended in a gas stream. The studies are part of the Bureau's continuing research on synthetic liquid fuels. The size and size-distribution of agglomerates as they exist when the gas reaches the filter was determined by using a membrane filter in conjunction with a dust count under a microscope. A membrane filter is a cellulosic sheet about 150 microns thick containing millions of holes per square centimeter--holes of uniform diameter that run directly through the sheet without interconnection.

Jan 1, 1960

By Warren M. Mahan

A rotary kiln process was developed by the Federal Bureau of Mines to produce consistently an iron product containing 3 to 7 percent nickel. Cuban laterite and serpentine ores were smelted in a gas-fired batch-rotary kiln) 5 feet in diameter and 9 feet long. The metal contained 2 to 4 percent carbon, with little or no silicon, and could be produced on a large scale with modest capital investment. A total of 121 tests was run using this procedure. The tests were conducted with a maximum temperature of 2,625° F., using linings of firebrick containing 40 to 70 percent alumina. Slags in the kiln were acid to neutral. The material in each batch passed through three stages: (1) Sponge metal, (2) carburization, and (3) balling and meltdown. Half the tests were made while firing the kiln with atmospheric-temperature air; the remainder were fired with preheated air. Tests showed that preheated air decreased fuel requirements, dust losses, and reducing agent, and increased the capacity of the kiln.

Jan 1, 1960

By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By M. G. Zabetakis

This publication describes an investigation conducted by the Federal Bureau of Mines regarding the cause of an explosion of a dephlegmator or fractionating column at the Cities Service Oil Company Refinery, Ponca City, Okla., January 22, 1959. The column was that used with the refinery's No.1 Dubbs Coker. The explosion caused the death of an employee of the refinery and resulted in extensive damage to the refinery and to nearby property. The Bureau's study of the explosion began January 26.

Jan 1, 1960

By D. Bienstock

The Fischer-Tropsch synthesis is practicable in a reactor where the exothermic heat of reaction is removed by circulating large quantities of recycle gas through a catalyst bed of high-voids content. At an hourly space velocity of 1100, the feed gas, a mixture of 1.5 parts hydrogen to 1 of carbon monoxide, was converted 90 percent, producing hydrocarbons predominantly in the gasoline range. At these conditions a recycle-to-fresh gas ratio of 40:1 was enough to give excellent temperature control with a pressure drop of 1.5 p.s.i. per foot of bed using a steel catalyst in the form of lathe turnings. Steel parallel plates, although offering lower resistance to gasflow, were less reactive and less durable. INTRODUCTION The Federal Bureau of Mines has been engaged in a research and development program since 1944 on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a synthesis gas--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va.; and the synthesis of gasoline by catalytically reacting the carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By J. L. Konchesky

The technical feasibility of gasifying powdered, noncoking, low-rank coal with steam in an externally heated tube has been demonstrated. The tube, 112 ft. of alloy-steel tubing shaped into a helix, served as an electrical conductor of electricity used for heating. The effects of the following variables were studied: Residence time of coal in reactor, average reaction temperature, steam concentration, and rank or geologic age of coal. Reaction pressure was maintained in the range 19-26 p.s.i.a. High carbon conversions and large yields of synthesis gas were obtained with low-rank coal. In one test, for example, about 88 pct. of the carbon in a subbituminous C coal was gasified at 1,910* F. with a residence time of 1 sec. The gas contained 58 pct. H2, 19 COD 15 CO, and 3 CH4; the yield was 30 cu. ft. (at 32' F. and 14.7 p.s.i.) of synthesis gas (CO + H2) per pound of dry coal.

Jan 1, 1960

By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By A. D. Hahn

The Federal Bureau of Mines examined ilmenite-bearing sands in southern Texas as part of a program to discover sources of supply for the domestic titanium industry. Deposits were examined from May 1956 through January 1959 in the outcrops of sandstone beds in the Jackson group of Eocene formations in Lee, Burleson, Fayette, and Starr Counties on the Gulf Coastal Plain; in alluvial valley fill in Brewster County in southwest Texas; in the sand beaches of Matagorda Peninsula and the Galveston, Padre, and Brazos Islands--part of the offshore chain of barrier islands along the Texas coast; and in unconsolidated sediments in Willacy County on the Rio Grande delta in the southeast Texas.

Jan 1, 1961