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By H. G. Wolfhard

The propagation of explosions through short cylindrical channels has been investigated by the Bureau of Mines. In the experimental apparatus set up by the Bureau, a single such channel formed a connection between a small explosion vessel in which a gaseous explosion was initiated and a larger, partly enclosing, explosion vessel filled with suitable gaseous mixtures; the larger vessel permitted observation to determine if an explosion was induced therein by mass, energy, and species transfer through the channel, as a result of tie initial explosion, It has been found that transmission of flame through to channel is not an essential to induce the second explosion, for hot gases from an extinguished explosion are able to ignite cold combustible mixtures in the larger vessel. The schlieren patterns of flames or hot burned gases emerging from a channel into the explosion chamber were photographed. These show, in most instances, that vortexes of hot gas ejected from the jet into the cold explosive mixture are responsible for ignition. The study has practical significance in problems of rendering electrical equipment safe for use in potentially flammable atmospheres, INTRODUCTION The propagation of flames through cylindrical or annular channels has practical importance in flameproofing electrical equipment and for flame traps. Much practical work has been done to determine the minimum safe breadth of flanges and the maximum safe gap between the flanges that will permit venting an electric motor without allowing flames to pass.

Jan 1, 1959

By K. K. Kershner

The purpose of this investigation was to develop methods, on a laboratory scale, for recovering tin from Bolivian metallurgical slimes. Petrographic and chemical analyses were made of slime ore fractions from several well-known tin operations. High percentages of the total tin were volatilized as chlorides at temperatures below 600° C. Under optimum conditions reaction rates were relatively rapid, and the chloridizing reaction approached completion. Owing to the low temperatures involved and the high yields of tin, the process was considered to have possibilities for treating Bolivian slimes on a commercial basis. ACKNOWLEDGMENTS Appreciation is hereby extended to the Patino Mines and Enterprises, Inc., of Bolivia, for supplying slimed tin ores that were used in the experimental work. This company has since been nationalized.

Jan 1, 1959

By E. C. Tarpley

An acid-extraction procedure developed in Germany for determining mineral matter in coal was investigated by the Bureau of Mines to determine its application to American coals. It was found to be suitable for all ranks of coal from anthracite to lignite if modified slightly for coals containing considerable quantities of calcium compounds, such as calcite or calcium humate. The precision of the method is satisfactory, and the results are probably closer to the true content of mineral matter than those obtained by empirical formulas. The method requires considerably more analytical data than the Parr or approximation formulas but is no more time consuming than obtaining the necessary data for the King, Maries, and Crossley formula (theoretically the most comprehensive empirical formula used). An appendix to this report includes a detailed description of a recommended procedure.

Jan 1, 1959

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 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 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 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