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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 G. V. Sullivan

This report describes an investigation by the Bureau of Mines of flotation techniques for the recovery of chromite from fine-grained disseminated ores. Reported work on the concentration of chromiferous materials shows that flotation has been applied almost exclusively to slime-free pulps. Therefore, chromium recoveries that could be obtained by flotation were related to the amount of slime rejected. However, results of recent studies by the Bureau of Mines showed that des liming is not a requisite to selective concentration of chromite. Laboratory-scale tests on seven ore types from the more important chromium-bearing areas of the Pacific Northwest showed flotation to be technically feasible for treatment of all but one of the samples. Concentrate grades were affected more by the composition of the chromite mineral than by the grade or character of the ore. Test results from three of the samples showed that, without prior desliming of the pulp, 78 to 91 percent of the chromium could be recovered in concentrates of 90 percent or more chromite; two samples responded to similar treatment, resulting in concentrates of more than 80 percent chromite with recoveries of 85 and 89 percent chromium. One sample of mill products, subjected to severe weathering, required removal of the primary slime to obtain a concentrate of 65 percent chromite with only 75 percent chromium recovery.

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 E. J. Ostrowski

The Bureau of Mines experimental blast furnace, Bruceton, Pa., was operated to determine the feasibility of replacing part of the burden coke requirements with solid fuels injected directly into the smelting zone. This report describes preliminary experiments and information resulting from such an interchange. These experiments were made on an all-sinter burden, using two parts sinter to one part fuel. Anthracite fines were injected intermittently into the smelting zone of the furnace by compressed air through auxiliary tuyeres. The interval between injection periods ranged from 5 to 15 minutes. A maximum of 28 percent of the stock column coke bur-den was replaced. This percentage replacement caused furnace malfunction, but the overall percentage of these experiments indicated that 20 to 24 percent of the coke requirements could be replaced in this way. The metallurgical coke consumption was decreased by as much as 377 pounds (25.3 percent) per ton of pig metal produced. Buckwheat anthracite No.4 was used in this experiment; however, such solids as bituminous coal or coke fines also could be used. The frequency as well as the quantity of solid fuel injected has a direct bearing on furnace performance.

Jan 1, 1960

By A. J. Barry

Two methods of testing anchorages of headed expansion-type mine roof bolts were investigated by the Federal Bureau of Mines to determine whether they are acceptable for general use. In both methods a load was applied to a tightened bolt with a hydraulic jack. A total of 80 tests, 40 using each method, was conducted in 4 test areas in 3 commercial coal mines. Electric resistance strain gages were used in all tests to indicate true bolt load as the bolt was tightened and when an additional load was applied with the hydraulic jack. The results indicate that: 1. The relationship between the true bolt load and the jack load will vary according to the test method until the two loads become equal. The bolt load-jack load relationship below this point can be determined only with strain gages. 2. The point at which the two loads become equal can be estimated by noting the load when the hardened washer becomes loose in one method, and when the bearing plate becomes loose from the roof in the other. It also can be approximated for either method of testing by noting the load when the first abrupt change in the slope of the jack load-bolt displacement curve occurs. 3. The anchorage characteristics of the test bolt can be determined from the data obtained from either method by examining the slope of the jack load-bolt displacement curve above the point at which the true bolt load is equal to the jack load.

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 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 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

By H. H. Heady

A naphtha obtained by destructive, recycle hydrogenation of crude shale oil, produced by gas-combustion retorting of Colorado oil shale, was found by the Bureau of Mines to contain 49.1 percent paraffins, 20.3 percent cycloparaffins, 7.8 percent olefins, and 22.8 percent aromatics. The naphtha contained only minor amounts of sulfur, nitrogen, and oxygen compounds. Compounds containing less than 5 carbon-atoms per molecule were removed by distillation before analysis. The paraffins where predominantly straight-chain compounds; n-Hexane was present in the largest quantity, and the other straight-chain paraffins decreased in amount as the molecular weight increased. The cycloparaffins, which contained both cyclopentanes and cyclohexanes, were evenly distributed throughout the boiling range. Although the naphtha had been produced by hydrogenation, it contained a small quantity of olefins. Straight-chain olefins with a terminal double bond comprised about two-thirds of these compounds. Among olefins with an internal double bond, those having trans configuration were present in three times the quantity of those in the cis form. In the aromatics all but one of the alkylbenzenes having nine or less carbon-atoms per molecule were identified; toluene was present in the greatest quantity. Only a few of the higher molecular-weight homologs were identified. The composition of the naphtha was computed from analyses of 105 narrow¬boiling distillation fractions. Volume, density, refractive indices, bromine number, and an ultraviolet spectrum were determined on each fraction. From these data the hydrocarbon-group composition of each fraction was estimated. A silica gel adsorption analysis was used to check the values of nearly one-third of the fraction calculated from physical-property data. Mass and infrared spectra were obtained on some fractions for identifying individual compounds or types of compounds, such as terminal olefins.

Jan 1, 1960

By G. L. Cook

The design of a dual-inlet system for a Consolidated model 21-103C mass spectrometer is described in detail. The system permits both high-mass and low-mass samples to be run by using a single instrument. The difficulties of using a single instrument for both purposes are given and a method of minimizing these difficulties through the use of the present design is discussed, After examining the experience of five years of use, the conclusions are that the bimodal operation is practical and the low-mass analyses had nearly the same precision as before the modifications to the instrument were made. In 1951, O'Neal and Wier.5/ published the first description of the modifications made to a mass spectrometer so that the spectra of hydrocarbons with molecular weights up to 600 could be obtained. Further discussion of the equipment of O'Neal appeared in 1953.6/ Also, Brown, Melpolder, and Young7/ described a parallel inlet system designed to reduce sorption effects at room temperature.

Jan 1, 1960

By E. G. King

Thermodynamic calculations involving the oxides of tungsten and molybdenum have been hampered by lack of accurate entropies and high temperature heat contents. This paper presents work by the Federal Bureau of Mines on new low-temperature heat-capacity data leading to the evaluation of the 298.15° K. entropies of tungsten dioxide and tungsten trioxide, as well as high-temperature heat contents (above 298.15° K.) of molybdenum dioxide, molybdenum tri-oxide, tungsten dioxide, and tungsten trioxide. Included are heats of fusion of the two trioxides. The heats of formation at 298.15° K. of these four oxides are tabulated as measured by Mah4 5/ of this laboratory. Included also are the 298.15° K. entropy of Mo02 measured by Kin 6/ of this laboratory, and that for Mo03 according to Kelley and King.7/ These basic data provide a consistent compilation from which to perform accurate thermodynamic calculations involving these compounds. No previous low-temperature- heat-capacity measurements have been reported for tungsten dioxide. Seltz, Dunkerley, and DeWitt8/ measured the low-temperature heat capacity of tungsten trioxide. The only previously-reported high-temperature heat-content measurements for any of the oxides were conducted by Cosgrove and Snyder,9/ who measured molybdenum trioxide to 1,300° K.

Jan 1, 1960

By W. M. Mark

This investigation was undertaken to develop methods to improve the quality of titanium sponge produced by the Bureau of Mines modification of the Kroll magnesium reduction process. Research revealed that by systematic elimination of detrimental impurities introduced with the raw materials and by improved handling and processing techniques, high-quality ductile titanium with a hardness of less than 110 B.h.n. (Brinell hardness number) can be produced consistently. This improvement was accomplished by helium (or argon) stripping of residual atmospheric and other dissolved gases from the titanic chloride, preliminary dehydration of crude titanium sponge, and careful regulation of the titanium tetrachloride (TiC14) feed rate to the reactors.

Jan 1, 1960