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By G. W. Birge, D. E. Wolfson, J. H. Lynch

This report by the Federal Bureau of Mines describes the carbonizing properties of coals from the principal beds in Boone County , W. Va . Results are given for samples of coals from No. 5 Block , Stockton - Lewiston , Coalburg , Winifrede , Chilton , Hernshaw , Cedar Grove , Alma , and No. 2 Gas beds . Boone County coals rank as high -volatile A bituminous . Eighteen of the 21 samples tested contained from 3.3 to 7.9 percent ash and 16 of the samples contained from 0.6 to 0.9 percent sulfur . Two samples from the Alma and No. 2 Gas beds , the lowest stratigraphically of the seams tested in Boone County , contained from 1.4 to 2.7 percent sulfur . Most Boone County coals yield

Jul 1, 1960

By Carl Rampacek, W. A. McKinney

The feasibility of leaching calcareous and siliceous oxidized copper ores by downward percolation with dilute acid was investigated in the laboratory and in a small continuous plant operated by the Federal Bureau of Mines . The crushed ore was leached in deep columns with solutions containing 1 or 5 percent sulfuric acid to dissolve the oxidized copper . Bench - scale laboratory tests on two calcareous ores from the same deposit indicated that a maximum copper extraction , about 72 percent , could be expected from heap leaching a feed as coarse as 1 inch . Laboratory tests on a siliceous ore showed that almost 70 percent of the copper could be extracted by leaching a 1 / 4 - inch feed . The bench - scale tests were supplemented by larger continuous runs wherein the copper was recovered from the leach liquors by precipitation on detinned scrap iron . Leaching the calcareous ore for approximately 10 days recovered 62 percent of the total copper . The sulfuric acid consumption was 9.6 pounds per pound of copper recovered . Treatment of the siliceous ore recovered 62.5 percent of the total copper in a 2.5 - day leach and the acid consumption was 3.7 pounds per pound of copper recovered . Cement copper products that assayed over 71 percent copper were obtained from the leach solutions by precipitation on scrap iron . The bench - scale and continuous tests demonstrated that downward percolation leaching of the calcareous ores was technically feasible but not economically practicable because of high acid consumption by the gangue . Leaching of the siliceous ore was rapid and the acid and water requirements were nominal . The downward percolation leach procedure is simple and requires a minimum of plant equipment .

Jul 1, 1960

By F. R. Cattoir, D. H. Baker

Fused - salt electrorefining has been successfully applied to the purification of vanadium metal . The electrolyte used in this refining technique was sodium chloride to which had been added 3 to 6 percent vanadium as vanadium dichloride . The average deposition current efficiency was 91 percent . Oxygen and nitrogen , the impurities in commercially produced vanadium metal , were reduced by two - thirds of the amount contained in the feed material . Hardness of the vanadium- metal product was reduced from an initial 97 Rockwell B ( RB ) to a minimum of 35 Rg . The reduction of these impurities markedly improved the plasticity of the final product obtained by melting the crystalline cell metal into small ingots . These ingots could be given a 99 - percent cold reduction by rolling before edge cracking appeared . Growing interest in high - purity vanadium and the industrial need for purer metals and improved alloys for use under high temperatures and high speeds have demanded the elimination and/or control of impurities . Accordingly, research to eliminate or control the undesirable impurities has been expanded .

Jul 1, 1960

By R. W. Stahl

"This study by the Federal Bureau of Mines was confined to pillaring with continuous mining machines and to mines where total extraction is practiced. Many different conditions and practices in as many coalbeds as possible in Pennsylvania were observed.Pillar extraction or pillaring can be the most productive part of coal mining if done properly; but it also can be the most dangerous if done improperly.Because of the need for more careful planning before and caution during pillaring, many mining companies resort to the undesirable practice of stumping or hogging of pillars with subsequent unnecessary waste of valuable natural resources. Pillaring can be done at reasonable cost and safely, as proven at many mines where complete extraction is practiced and enviable cost and accident records are maintained.Although continuous mining machines are bulky and sometimes difficult to maneuver, they have been used with great success in pillaring. Occasionally, however, a machine is caught, or men are injured by a fall during pillar recovery. This Bureau survey was conducted to ascertain how safe and successful pillaring (especially the removal of final stumps in lifts or the final stump of a pillar), is accomplished in some mines, while others have considerable difficulty under similar conditions.The Bureau hopes the information to be presented in this publication will prove beneficial to those who wish to recover more pillar coal and to improve their accident record during such procedures."

Dec 1, 1959

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

"Investigations in the Federal Bureau of Mines Experimental coal mine near Pittsburgh, Pa., have shown that high-expansion foam containing at least 0.2 ounce of water per cubic foot of volume is effective in controlling exper-imental underground coal, oil, or wood fires. Some of the fires were extinguished, but more of the coal and wood fires were brought under enough control to permit direct attack with water or other extinguishing agent or loading the hot material into cars. The largest controlled experimental fire, which burned about 5 hours before attack, was in a coalbed 5 feet wide, 10 inches thick, and 100 feet long. The greatest distance foam was transported to control a fire was 1,010 feet.An incipient fire should be attacked promptly with water, rock dust, or other approved and readily available extinguishing agents. Where heat, roof falls, and smoke prevent direct approach, the more involved procedure of using foam may be advantageous. The effectiveness of the foam in controlling a deep coated fire of considerable extent H,vet to be proved by actual trials in aSome hydrogen, carbon monoxide, and methane gases are generated when a fire is attacked with foam. Calculations showed that in experimental fire tests an explosive mixture could form; however, this would occur only within a narrow range of combustible gas-air mixtures not likely to be found in practice. The principal explosion hazards are due to generation of gases by the foam, localized build-up of normally liberated methane, and volatiles liberated by the coal during heating. The quantity of combustible gases generated by the action of the foam on the fire is about the same as that when an equivalent amount of water is applied."

Mar 1, 1960

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 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 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 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 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 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 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