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By Gerald W. Elger

The Federal Bureau of Mines developed a modification in the conventional Kroll process for preparing high - purity hafnium metal . This modification involved the partial replacement of magnesium by sodium in the batch reduction of purified hafnium tetrachloride to sponge metal . The raw tetrachloride was purified either by thermal degassing of the volatile contaminants to the atmosphere or by fused- salt treatment . In the fused- salt treatment , the tetrachloride was contacted with molten alkali chlorides to remove the impurities . The reaction byproducts were removed from the metal by heat treatment in an evacuated furnace . The metal sponge was consolidated by melting into buttons or ingots , which were analyzed for impurities . The purity of the metal prepared by the modified process is superior to that of the metal produced by the conventional method . The hafnium metal was comparable to crystal - bar hafnium except for the oxygen content , despite the abnormally high impurity concentrations in the raw tetrachloride . Several ingots were successfully cold - rolled to sheet .

Jul 1, 1960

By P. L. Woolf, J. P. Morris, E. Foerster, G. R. Zellars

Measurements of vapor pressure can be used to determine the thermodynamic activities of the components of metallic solutions . The determination of activity by this method requires accurate values for the vapor pressure of the pure component and for its partial pressure above the alloy solution . This investigation was conducted to measure the vapor pressure of liquid manganese for use in future studies of the activity of manganese in various liquid alloys . In related investigations in the Bureau's Pyrometallurgy Laboratory , vapor pressures of copper , iron and nickel have been measured and activit 4 5 6 have been determined in the iron- copper and iron- nickel systems . Difficulties were experienced with manganese which were not encountered in the previous investigations . Manganese oxidizes readily and greater care was needed to maintain an oxygen- and moisture - free atmosphere in the furnace . In addition , liquid manganese wet the refractories and there was a tendency to foam and splash on introduction of the carrier gas . Because of these difficulties several variations in the experimental procedure were studied . These were first tested with silver which has a vapor pressure of the same order of magnitude as manganese but is relatively inert at high temperatures . Although no significant changes in the original procedure resulted from this work, considerable data were obtained for silver and have been included in this report . Bauer and BBrruunnnneerr7/ have reported the only extensive investigation of the vapor pressure of liquid manganese . However , their results are not consistent with the data obtained by McCabe and Hudson for solid manganese . Measurements of the vapor pressure of silver have been reported by McCabe and Birchenal1,2/ Schadel and Birchenall , 10/ Harteck , 11 / Fischer , 12/ and von Wartenberg.13 / Generally , these investigators conducted their measurements at lower temperatures than were used in this study .

Jul 1, 1960

By Michael G. Zabetakis, Glenn H. Damon, Joseph A. Herickes

The flammability and explosibility of unsymmetrical dimethylhydrazine ( UDMH ) were investigated by the Federal Bureau of Mines to evaluate hazards associated with commercial application of this material as a missile fuel . This program included the following determinations : 1. Temperature limits of flammability in air at one atmosphere pressure ; 2. limits of flammability at selected elevated temperatures and pressures ; 3. 4 . 5. spontaneous ignition temperature in air at one atmosphere and at 200 pressure per square inch gage ( p.s.i.g. ) initial pressure ; spontaneous decomposition temperatures in nitrogen at one atmosphere and at 200 p.s.i.g .; shock sensitivity over a temperature range from about ( ca. ) 25 ° to 50 ° C .; 6. shock sensitivity of reference propellants ( hydrazine , nitromethane , methyl acetylene , etc. ) ; 7 . shock sensitivity of UDMH plus small amounts of selected metal catalysts . Part of the corresponding data was obtained for a mixture of unsymmetrical - dimethylhydrazine and diethylenetriamine ( U - DETA) .

Jul 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 A. L. Engel

This publication describes further research by the Federal Bureau of Mines in beneficiating domestic manganese ores. The ores selected for treatment were typical of many manganese deposits in California and Nevada in that they have not been economical to mine because they are low grade or contaminated with siliceous minerals and are not amenable to physical concentration.3 4/ It would be desirable to develop a simple treatment method resulting in nearly complete extraction of manganese from these ores and applicable to small-scale operations. Sulfation reduction appeared to be such a method. The studies reported in this publication were directed toward sawdust or lignin-sulfonates as reducing agents. Sawdust, as waste from lumbering, and lignin-sulfonates, byproducts of woodpulp papermaking, are comparatively cheap and may be available in areas where manganese ores are found. Sugar, oils, and coal were also tried as reducing agents.

Jan 1, 1960

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

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 H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960

By V. B. Dale

This paper is one of a Federal Bureau of Mines series covering the mineral resources of the Nation. It briefly describes most of the tungsten deposits in Cochise, Pima, and Santa Cruz Counties, Ariz. Most of the descriptions are from field examinations by the two senior writers, prior to July 1957. Wolframite first was identified in Arizona in 1896 by W. P. Blake, Territorial Geologist. Tungsten mining began about 1900 in the Little Dragoon deposits of Cochise County, and about 1901 in Las Guijas district of Pima County. The price history of tungsten is an erratic one; consequently, production has been erratic. Prices rise during wars and periods of national preparedness. Production of tungsten ore was stimulated greatly by a Government purchasing program, announced on May 10, 1951, wherein the Government agreed to purchase standard-grade tungsten concentrates at $63 per short ton unit5/ for 5 years or until 1,468,750 units were purchased. This was later increased to 3,000,000 units, and after this amount had been purchased in June 1956, the purchase of an additional 1,500,000 units was authorized. Government purchase, however, was suspended in December 1956 before completion of this latter program, and the price of tungsten concentrates declined sharply. The price had dropped to $15 per short ton unit, duty extra,6/ by the last part of July 1957.

Jan 1, 1960

By Joel N. Van Sant

The rapidly expanding economy of the West, with its growth of heavy industry, and increased steel production, is primarily responsible for the refractory clay industry's concern over the adequacy of the clay supply in States of the Great Plains and Rocky Mountains. Hence, the investigation by the Federal Bureau of Mines of the occurrence and use of refractory clays in North Dakota, South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona has been encouraged by the major consumers and producers of this commodity. The Wyoming investigation is a part of the national program devised to close gaps in the domestic supply of specific types of clays to determine their characteristics and properties and to provide information that will assist the refractory-clay industry. Forty-two locations of clay-bearing rock in 17 areas in Wyoming were examined (fig. 1). Location 3 was not examined during this survey. Its description was taken from an earlier report. Locations 20, 21, and 22 were previously reported but were, also, examined by the Bureau. No samples were collected from these locations because field examination indicated that the shales were not refractory grade. The Hulett, Aladdin, and Newcastle areas are discussed in the section on the Black Hills district; the other 14 areas are described separately.

Jan 1, 1961

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By J. B. Gayle

The rate of oxidation of coals with nitric acid has been used by earlier investigators4 5 6/ for determining fusain and for studying petrographic composition. These workers accumulated considerable evidence indicating that, for coals ranging from lignite to low-volatile in rank, the method gives values for fusain that agree satisfactorily with those obtained by optical methods. One group5/even concluded that, when discrepancies are noted between results obtained by chemical and microscopic methods, the results based on the oxidation reaction are probably the more reliable. Unfortunately, after concluding that the method was valid, most of these workers apparently lost interest. As a result, no attempt to exploit or apply the method to problems of utilization has been reported. Recent studies of the influence of inert petrographic constituents on the properties of cokes made from various coals7/ have indicated a need for additional means of characterizing coals and blends used for carbonization.

Jan 1, 1960

By Jack D. Ramsdell

Electrorefined, magnesium-reduced, and sodium-reduced titanium samples were evaluated for recrystallization behavior, effect of cold rolling on tensile properties, and bend ductility. Curves were determined for the softening of 2.5 to 80 percent reduced cold-rolled metal that was annealed over a temperature range of 300° to 800° C. Upon annealing, coarsening of the grains was found to occur for reductions in thickness of less than 20 percent in titanium made by all three processes. The presence of metallic impurities greatly inhibits coarsening for reductions in thickness below 20 percent, but for reductions in excess of 20 percent grain size is essentially constant at each annealing temperature. The three grades of titanium did not harden excessively from cold rolling; both tensile and bend ductility were good for reduction in thickness up to 80 percent. Upon annealing, softening occurs between 400° and 600° C., and, based on microstructure and property studies, full annealing is accomplished after 30 minutes at 700° C. for the magnesium-reduced and electrorefined titanium and at 800° C. for the sodium-reduced titanium.

Jan 1, 1960

By James S. Browning

Heavy liquids have been used to separate minerals of different specific gravities for many years.4 5 6 7 8 9/ The method permits substantially quantitative evaluation of a variety of minerals and requires much less time than the usual methods of chemical analysis. This Bureau of Mines investigation was conducted to determine the applicability of heavy liquid mineral separation to the evaluation of certain spodumene and kyanite ores, prepared mixtures, and plant products. After careful standardization of the particular mineral and associated gangue, estimates of chemical analyses could be obtained from results of heavy liquid separations.

Jan 1, 1960

By C. A. Frenzel

Extensive spectroscopic data are needed in making reliable vibrational assignments for use in calculating thermodynamic functions of polyatomic molecules. The fundamental vibrations of organic molecules may be observed at any wavelength from 2.5 to 200 microns (micron = µ = 10-4 centimeters), but most often in the region from 3µ to 50µ. Raman spectra generally cover the range in which fundamental vibrations occur, but equally important infrared spectra usually are not measured at wavelengths longer than 25µ. This limitation results because most infrared spectra are determined for analytical purposes, which seldom require information outside the region 2µ to 25µ. Measurements of infrared spectra in the range 15µ to 35µ recently were begun by the Bureau of Mines to obtain data needed in making vibrational assignments. This report presents the spectra of the following thirteen compounds: Tetrahydrofuran, 1-methylpyrrole, piperidine, 2-methylpyridine, 3-miuthylpyridine, 2-propanethiol, cyclopentanethiol, 2-methyl-2-butanethiol, 3,3-dimethyl-2-thiabutane, cyclohexanethiol, cyclopentyl-l-thiaethane, 2,4-dimethyl-3-thiapentane, and hexamethyldisiloxane.

Jan 1, 1960

By R. L. Montgomery

Heats of solution of yttrium chloride and oxide in hydrochloric acid were measured by Bureau of Mines researchers. Using the heat of combustion of yttrium mentioned in the literature, the Bureau calculated the heat of formation of yttrium chloride to be -239.16 + 0.50 kcal./mole. The Bureau experiments gave evidence that the heats of solution of yttrium chloride from the literature are mostly too low because of water and/or oxychloride impurities. Heat of combustion of yttrium (8)3/ and its heat of solution in hydrochloric acid (2, 14) have been measured. The earlier heat of solution measurement (2) is unreliable because of possible potassium contamination (4). Heat of solution of yttrium chloride has been measured by three researchers (3, 9, 15), who obtained widely different results. Spedding and Flynn (14) report the heat of formation of yttrium chloride as -232.69 kcal./mole from their solution studies. The present work was designed to check the reported heats of solution of yttrium chloride and to determine the heat of solution of yttrium oxide. The latter measurement would allow the results of solution and combustion data for yttrium to be intercompared.

Jan 1, 1960

By J. H. Field

Results of studies by the Federal Bureau of Mines on a pilot-plant scale for removing hydrogen sulfide and carbonyl sulfide from gas mixtures by the hot carbonate system are given in this publication. Gases containing up to 10 pet. hydrogen sulfide and 48 grains carbonyl sulfide per 100 cu.ft. were treated. In most tests carbon dioxide also was present and was removed simultaneously with the sulfur compounds. Because the rate of absorption of hydrogen sulfide is much more rapid than that of carbon dioxide over a wide temperature range, selective removal of hydrogen sulfide occurred in the bottom section of the absorber near the point of gas entry. Hydrogen sulfide was removed to pipeline specifications with carbonate solutions by using split-stream flows in the absorber and regenerator.

Jan 1, 1960

By T. A. Henrie

The Federal Bureau of Mines has investigated methods of sodium reduction of titanium chlorides to produce high purity titanium metal (14).4/ This investigation was made to obtain a better understanding of the reactions involved in sodium reduction of titanium chlorides and was part of the Bureau's activities toward improving the technology of titanium. Theoretical and experimental evidence show that sodium reduction of titanium tetrachloride occurs by stepwise reactions. The first stage reduction between sodium vapor and vapors of titanium chlorides produces titanium di-and trichlorides which subsequently condense with sodium chloride to form a salt mixture. The second stage reduction takes place in the condensed salt mixture between sodium and titanium subchlorides. Final reduction is a heterogeneous reaction between two separate phases, the a phase which consisted of sodium dissolved in sodium chloride and the ß phase titanium subchlorides dissolved in sodium chloride. The mechanism of the heterogeneous reaction between these phases is electrochemical in nature. The model proposed is a galvanic reaction at the interfacial region.

Jan 1, 1960