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 Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation.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

By A. D. Hahn

This report describes reconnaissance by the Federal Bureau of Mines of titanium-bearing sandstone in Kemper County, Miss. The purpose was to determine the ilmenite, rutile, and associated heavy-mineral content of black-sand-bearing Eocene deltaic formations" The investigation was part of a survey of titanium resources of the United States. Ilmenite (FeTi03), an iron-titanium oxide, is the major titanium-bearing mineral consumed in the titanium pigment industry. Rutile (Ti02), titanium oxide, is used mainly in producing welding-rod coatings and titanium metal. The fieldwork was conducted during the first half of November 1959. Seven holes, totaling 304 feet of bore, from which 64 samples of cuttings were taken, were drilled in the north-central part of the county; and two holes, totaling 172 feet of bore, from which 34 samples of cuttings were taken, were drilled in the southeastern part.

Jan 1, 1961

By Paul L. Campbell

Investigations by the Federal Bureau of Mines of methods of upgrading tar obtained by low-temperature carbonization of lignite showed that ß,ß?-oxydipropionitrile, ß,ß?-iminodipropionitrile, and ß,ß'-thiodipropionitrile were effective solvents for extracting aromatics (aromatic hydrocarbons plus polar compounds) from coal-tar neutral distillate fractions. Batch extraction showed that these solvents extracted approximately the same percentage of aromatics from various neutral oil fractions boiling between approximately 170° and 350° C. In continuous countercurrent extractions using oxydipropionitrile and iminodipropionitrile, approximately 30 to 35 vol.-pct, and 65 to 70 vol.-pct, of the aromatics in 170° to 350° C. neutral distillate oil were extracted at room temperature when solvent-to-oil ratios were 2:1 and 12:1, respectively. As the concentration of aromatics in the neutral distillate oil fraction decreased, the capacities and, to some extent, the selectivities of these solvents for the remaining aromatics decreased. Aromatics were isolated from the extracts and the solvents recovered by washing the extract fractions with a low-boiling paraffinic hydrocarbon such as heptane, using hydrocarbon-to-extract ratios of at least 2:1. The heptane wash removed most of the aromatics but only part of the polar compounds (compounds containing oxygen, sulfur, and nitrogen) from the extracts. The recovered oxydipropionitrile and iminodipropionitrile, containing polar compounds, were effective in extracting aromatics from neutral distillate oils. The contaminated solvents showed essentially the same capacities and selectivities as the pure solvents.

Jan 1, 1961

By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

By W. A. Calhoun

The purpose of this investigation was to develop economical mineral dressing processes for removing objectionable quantities of impurities, such as quartz and pyrite, from refractory clay deposits in east central Missouri. The presence of excessive quartz in these clays causes crazing. Pyrite causes bloating and unsightly dark blobs on the surface of fired refractory brick. The iron concentration in the proper state of oxidation may also act as nucleation centers for carbon crystal growth which can result in bursting of the refractory. Numerous deposits, representing a very large tonnage, have been examined and prospected by various refractories companies and found to contain impurities in objectionable quantities. Upgrading these clays would greatly extend our reserves of high-quality refractory clays. Wet-tabling and wet-cyclone concentration were found to be effective for removal of impurities from clays. Of the two methods, wet-cyclone concentra¬tion would be cheaper and more effective. Although wet-tabling improved the refractory properties of each clay, beneficiation by wet-cyclone produced clays of superior quality. Clay recoveries by wet-cycloning ranged from 56.1 to 81.8 percent of the weight of the crude samples, and the beneficiated clays contained from 71.9 to 94.4 percent of the total alumina. The pyrometric cone equivalent (PCE) was increased from 1 to 3 cones by wet-cycloning. The beneficiated clays also met the reheat shrinkage requirements on refiring to 1,400° C. Missouri is one of the major domestic sources of fare clay. In addition to deposits of high-grade refractory clays, there arc many deposits that contain small percentages of impurities, which render the clays unfit for the production of high-heat-duty firebrick. Development of methods to beneficiate these submarginal clays to usable materials would greatly increase commercial fire clay resources.

Jan 1, 1961

By W. L. Hunter

The research on this report was conducted to obtain information on the feasibility of producing ferro chromium of varying silicon and carbon contents from domestic chromite. Concentrates from the Mouat deposit were chosen because they typify the chromite found in the Stillwater complex, the largest domestic reserve, and are similar in composition to other extensive North American and foreign deposits. Batch-smelting tests designed to produce high-, medium-, and low-carbon ferrochromium were made in single phase and three-phase, electric-arc, steelmaking furnaces. Agglomeration studies were made in a rotary kiln. Continuous smelting tests were made to yield data on the production of high-carbon ferro chromium and low-carbon ferrochromium-silicon. The carbon content of high-carbon ferrochromium was lowered to the medium-carbon range by oxygen injection. Mouat stockpile concentrates were nodulized in a gas-fired rotary kiln using quartz, limestone, and fluorspar additions in the proportion necessary to flux the slag. The nodules were smelted in a continuous test using coal, coal char, and mixtures of the two consecutively as reductants.

Jan 1, 1961

By R. S. McClain

The Federal Bureau of Mines investigated residues from aluminum plants, to determine if carbon could be removed by flotation while recovering fluorine and aluminum compounds for recycling to the reduction process. This publication summarizes studies on samples representing three types of plant waste products, supplied by three aluminum-producing companies. Samples of flue dust, pot skimmings, and pot linings from the various plants all responded to a simple turpentine flotation scheme to reject 90 to 97 percent of the carbon. Aluminum compound recoveries ranged from 42 to 94 percent on the flue dust, were about 95 percent on the pot skimmings, and ranged from 75 to 89 percent on the pot linings. Fluorine recoveries from the same samples ranged from 35 to 63, 92 to 95, and 77 to 86 percent, respectively. The pot linings contained soluble salts of aluminum and fluorine which were recovered by precipitation with sodium aluminate and carbon dioxide gas. Composites of residues from each plant responded to flotation much the same as the individual samples. Aluminum is produced by the electrolysis of alumina in a molten cryolite bath. The electrolytic reduction cell consists of a carbon-lined box containing a pad of molten aluminum which serves as a cathode, a carbon anode, and an electrolyte of molten cryolite in which the alumina is dissolved. Alumina is reduced to aluminum at the cathode, and carbon is oxidized at the anode.

Jan 1, 1961

By M. A. Hammer

In this study by the Federal Bureau of Mines Pennsylvania anthracite from the Eastern Middle field was oxidized by concentrated nitric acid at steam-bath temperature for 24 to 1,000 hours. The quantitative data obtained include yields of nitric-acid soluble and insoluble products and the distribution of carbon and ash in each. The acid-insoluble residues were examined for solubility in aqueous sodium hydroxide. With a sodium hydroxide concentration of at least 1 normal, a portion of the residue could be extracted in the form of a true solution. With lower alkali concentrations, peptization occurred. Alkali solubility of the residue increased with length of oxidation. However, when expressed in percentages of original coal weight, the alkali solubility remained essentially constant after 192 hours of oxidation. This suggests that the alkali-soluble products are converted to acid-soluble products at the same rate as the original coal substance is converted to alkali-soluble material. Microscopic observations of the peptization of the acid-insoluble residues revealed a gross micellar physical structure. The action of nitric acid is apparently not restricted to the surface of a coal particle. The acid penetrates the particle through the pore structure, dissolving some of the ash and altering the bonds between the coal micelles. The bond alteration, as indicated by ultimate analyses, involves the physical and chemical adsorption of the components of nitric acid. Some of the altered bonds are not thermally stable; this instability is shown by the complete loss of peptizing ability when the acid-insoluble products are heated above 200° C. This loss is accompanied by the evolution of water, oxides of nitrogen, and hydrocyanic acid.

Jan 1, 1961