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By A. A. Cochran

Methods of preparing small heats of steel containing radioisotopes were developed, and the techniques of stripping film autoradiography were used to detect and study the carbide and sulfide phases in titanium-bearing steels. Metallography had revealed areas of titanium sulfide and ferrite or pearlite adjacent to areas of titanium carbide and ferrite, and unidentified, irregular phases at the boundaries between these two areas. Sulfur 35 was used to deter-mine the extent of the titanium sulfide inclusions, and carbon 14 was used to delineate the titanium carbide phase. Individual radioactive areas were located with a resolution of approximately 10 microns. A general background exposure that was not correlated with microscopically visible phases was observed in the carbon 14 autoradiographs. The evidence from both sulfur 35 autoradiographs and carbon 14 autoradiographs indicated that the unidentified inclusions were sulfides rather than carbides. INTRODUCTION The use of radioisotopes to facilitate the work at the Rolla Metallurgy Research Center was expanded in fiscal year 1959 when the Bureau of Mines authorized the installation of an intermediate-level radioactivity laboratory. Before this time, sealed cobalt 60 sources had been employed for radiography, but no tracer work was done. The primary objective of the first experiments conducted in the new laboratory was to supplement physical metallurgy investigations of selected problems in steel research.

Jan 1, 1962

By R. E. Perry

To develop new or improved flotation methods for beneficiating low-grade red iron ores, the Bureau made many bench scale and continuous anionic flotation tests on ferruginous sandstones and calcareous iron ores from the north-eastern part of the Birmingham, Ala., iron district. The ores contained about 21 to 36 percent iron, a to 11 percent lime, and 22 to 64 percent silica. Production of iron concentrates containing 48 to 52 percent iron was technically feasible in batch tests, and the iron recoveries ranged from 85 to 92 percent. In continuous tests 49 to 51 percent iron products were obtained with 80 to 90 percent recovery.

Jan 1, 1962

By Richard D. Graves

Pitch from low-temperature carbonization of bituminous coal was hydrogenated at cracking conditions in a continuous bench-scale unit to produce low-molecular-weight oils and tar acids. The pitch contained 15.6 pct benzene-insoluble material, 4.0 pct hexane-soluble oil, and 80.4 pct asphaltene by weight. At 475° C, 7,500 psig, and 1.5 hours residence time, hydrogenation products, based on the weight of pitch, were about 36 pct oil boiling below 325° C, 24 pct hexane-soluble heavy oil, 17 pct asphaltene, 1 pct benzene insolubles, and 12 pct hydrocarbon gases. The yield of tar acids boiling below 250° C was 4.3 pct, and the yields of C6 to C8 paraffins, naphthenes, and aromatics were each less than 1.0 pct. The yield of tar acids was within the range of yields obtained by hydrogenation or high-temperature carbonization of bituminous coal (2 to 5 wt pct). Yields of oil boiling below 325° C increased with increased residence time or temperature. There was little or no effect of residence time on yields of alkali- soluble material which contained tar acids. Yields of hydro-carbon gases increased markedly with an increase in temperature from 475° to 500° C. Lowering the hydrogen pressure to 4,500 psig resulted in yields similar to those obtained at 7,500 psig.

Jan 1, 1962

By Raymond W. Hiteshue

To aid in designing a continuous system for evaluating processes for converting coal to high-Btu gas] the Bureau of Mines determined the amenability of various coals and a char to hydrogasification at 800° C and 6,000 psig using a molybdenum catalyst. A lignite from Rockdale, Tex., an hvCb coal from Rock Springs, Wyo., a char from the low-temperature carbonization of the latter, an hvAb coal from Pittsburgh, Pa., and an anthracite from Luzerne County, Pa., were selected. Highest yields of gaseous hydrocarbons, 94 pet, based on maf feed, were produced from char, and lowest yields, 67 pct, were obtained from lignite. Hydrocarbon gases contained 82 to 92 pct methane, 8 to 15 pct ethane; and 1 to 3 pct propane.

Jan 1, 1962

By A. J. Forney

The hot-gas-recycle process, for the hydrogenation of carbon monoxide, was investigated in a 12-inch-diameter reactor. Initially because the distribution of gas was poor, hotspots developed in the catalyst bed. After the velocity profile of the gas flowing through the bed was studied, the method of packing the catalyst was altered. Because this change improved the distribution of gas, temperature control was excellent. The l2-inch-diameter reactor was operated successfully in the synthesis of gaseous and liquid fuels. When high-Btu gas was synthesized in two stages, parallel-plate assemblies of Raney nickel were almost as active as granular Raney nickel in the second reactor. The pressure drop through the second reactor, however, was reduced 90 percent by the use of these assemblies.

Jan 1, 1962

By Michael G. Zabetakis

Investigation of gas explosions usually reveals that the combustible gases have come from transmission and storage facilities or from natural gas or oil wells. However, combustible gases such as methane and hydrogen can derive from biological processes. Hazardous situations have been created in the past by the use of abandoned mines for the disposal of sewage and rainwater, by the interconnection of storm and sanitary sewers, by sealing the openings in manhole covers when repaving the roadway over a sanitary sewer, and by the construction of buildings over or near garbage fill areas without adequately providing for the release of combustible gases.

Jan 1, 1962

By James A. Whelan

The Bureau of Mines sponsored research studies of variables in rotary drilling, done in the Department of Mineral Engineering, University of Minnesota. By studying carefully controlled drilling with good instrumentation, it was hoped to obtain a better understanding of rock failure during drilling and of the stresses in drill bits during drilling. Experimental procedures and equipment are described. From these studies it was concluded that 1. Thrust requirements, other things being equal, are proportional to the total length of cutting edge in the bit. 2. Data from penetrating a wedge into rock under thrust only are not directly applicable to rotary drilling. 3, In rotary drilling the initial wear on a bit greatly decreases penetration rate under any given set of conditions; however, after initial wear the effect of wear on penetration rate is reduced. 4. An increase in rotary speed increases the overall penetration rate but decreases the penetration per revolution. 5. An increase in thrust increases the overall penetration rate and the penetration per revolution. 6, Torque on a drill bit is proportional to both penetration rate and bit diameter. 7. For small-diameter holes full-hole drilling will save both drilling time and energy compared with pilot drilling followed by reaming; for large-diameter holes pilot drilling-reaming is advantageous in both respects,

Jan 1, 1962

Spectrochemical methods were developed to determine beryllium in the concentration range 0.0015 to 4.0 percent in siliceous mineral beneficiation products. Two methods are described. They are (1) a fusion-pellet-spark procedure (spark method) and (2) a sustaining alternating-current arc procedure (arc method). In the spark method the sample is fused with lithium tetra-borate and vanadium pentoxide. The resulting bead is crushed, mixed with powdered graphite, and briquetted. This is analyzed spectrographically using controlled high-voltage spark excitation. In the arc method the sample is diluted with germanium metal, graphite, and vanadium pentoxide. Weighed charges are packed into cupped graphite electrodes and subjected to excitation with a sustaining alternating-current arc. Vanadium serves as internal standard for both methods. Effects due to matrix variations in samples and standards are eliminated either by fusion with lithium tetraborate in the spark method or by dilution with germanium and graphite in the arc method. Beryllium determinations show deviations from accepted chemical values of approximately 5 and 8 percent for the spark and arc methods, respectively. Analyses can be made more rapidly by the arc procedure with a sacrifice in precision and accuracy. Either method can be applied to the determination of beryllium in silicate rocks.

Jan 1, 1962

By Frank A. Peters

This Bureau of Mines report is the second of a series of process evaluations planned to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. Included in these evaluations are recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The processes considered in this report are designed to extract alumina as aluminum chloride from calcined clay with 20 percent hydrochloric acid and to remove the silica residue by filtration. Iron is removed by one of the following processes: Isopropyl ether extraction, in which iron chloride is extracted before decomposing the aluminum chloride; gas precipitation, in which the aluminum chloride is precipitated with hydrogen chloride while leaving the iron chloride in solution; gas precipitation-isopropyl ether extraction, in which the aluminum chloride from precipitation is extracted with isopropyl ether, if necessary; caustic purification, in which a crude alumina is produced and then purified by a modified Bayer operation; or sinter purification, in which a crude alumina is produced and then purified by a lime-soda sinter operation. For plants producing 1,000 tons of alumina a day the estimated operating costs per ton of alumina are: [Isopropyl ether extraction process $ 65.09 Gas precipitation process 89.04 Gas precipitation-isopropyl ether extraction process 119.65 Caustic purification process 73.79 Sinter purification process 80.47] The estimated fixed capital costs per annual ton for these plants on a Marshall and Stevens chemical equipment basis of 240.0 are: [Isopropyl ether extraction process $229.03 Gas precipitation process 287.16 Gas precipitation-isopropyl ether extraction process 356.59 Caustic purification process 266.48 Sinter purification process 279.13]

Jan 1, 1962

By C. H. Riggs

This report describes the development, oil recovery, and potentialities of productive formations in the Hall-Gurney field, Russell County, Kans. It is presented as part of a general program to aid and promote increased recovery from petroleum reservoirs. The report is based on studies of well logs, drill cuttings, and oil-and water-production histories of individual wells and leases. The geological interpretations follow closely those in published literature with only slight local modifications. Oil and water analyses, made at a Bureau of Mines research center, were supplemented by many analyses obtained from oil-producing and service companies. The Hall-Gurney field, in south central Russell County, Kans., (fig. 1) was discovered in 1931 but was not developed extensively until 1941. By 1960 the rate of oil production from the field had declined to the extent that many wells were abandoned. In some areas natural productive forces have effected good recovery. However, in other areas inefficient waterflooding, both natural and accidental, has adversely affected recovery potentialities.

Jan 1, 1963

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Nicholas County, W. Va. It is one in a series describing coals suitable for producing metallurgical coke, either as mined or after beneficiation. Almost 5 million tons of coal were produced in Nicholas County, W. Va., in 1960, of which over 2.6 million tons were cleaned in eight preparation plants. It has been estimated that over 6 billion tons remained in the county as of December 31, 1960, in beds 12 inches and more thick.

Jan 1, 1962

By Louis A. Panek

Tests of mine-roof models in a centrifuge show that the suspension effect due to bolting a horizontally bedded mine roof with frictionless surfaces of contact between beds depends principally on the number of bolted beds and their relative flexural rigidities, provided that sufficient bolt tension is exerted to prevent strata separations at the bolt locations. Strata separations tend to occur in the unbolted roof mainly because the beds have unequal thicknesses. "Suspension effect" refers to the transfer of part of the weight of weaker or thinner beds to the flexurally more rigid beds by roof bolts or by any other means. The factors investigated were number of beds in the bolted unit, bed thickness, modulus of elasticity of beds, length of bolts, spacing of bolts across and along the opening, bolt load, and intensity of roof load. The general principles of behavior of the bolted roof beds are explained by an approximate theory. Model test data are used to validate the theory and to obtain an expression for the "suspension efficiency". As the suspension effect actually observed in the models is smaller than that predicted by the approximate theory, the suspension efficiency in general is less than unity. Mathematical expressions are obtained for (1) the change in roof bending stress due to the suspension effect, which is needed for design of a roof-bolting system, (2) the change of roof deflection due to the suspension effect, which may be useful for evaluating the effectiveness of a roof-bolting system, and (3) the bolt load or pre-load that is required to achieve the desired reinforcing effect.

Jan 1, 1962

By Lowell Stroud

This report is the third in a series presenting equilibrium vapor-liquid data for helium-bearing natural gases. The first two reports contained phase data for the gases processed for helium at the Bureau of Mines Amarillo and Exell, Tex., helium plants. The present report offers similar information for a lower-helium-content (0.75 mole-percent) natural gas to be processed in the Department of the Interior's long-range helium-conservation program. A windowed-cell apparatus was used to obtain 218 samples of equilibrium vapor and liquid phases at 73 experimental conditions ranging in temperature from -100° F to -275° F and in pressure from 100 to 500 psi. From the phase data, the condensation characteristics, helium solubility, and equilibrium-vaporization-coefficient data for helium, nitrogen, and methane were evaluated. The effect of using a. preliminary hydrocarbon trap upon the subsequent vapor-liquid compositions is reported. A brief comment regarding the composition effect of passing the gas through a gasoline-removal unit is also included.

Jan 1, 1963

By H. E. Peterson

This report revises an earlier publication by the Bureau of Mines on tungsten analytical procedures and expands the coverage by including appropriate procedures for the critical impurity elements that commonly occur in tungsten ores and concentrates (13).3 The basic methods described are not original, but many of the modifications to improve reliability and sensitivity were developed by the Bureau. Gravimetric and colorimetric methods currently used for the determination of tungsten in ores, mill tailings, and concentrates are described. Colorimetric procedures are preferred for low concentrations of tungsten, whereas either procedure is satisfactory for moderate concentrations. Conversely, a gravimetric method is preferred for the determination of tungsten in concentrates.

Jan 1, 1963

By R. O. Dannenberg

Exploratory research was conducted to ascertain the feasibility of recovering beryllium from Spor Mountain, Utah, ore by the sodium fluosilicate (Na2SiF6) method used industrially for processing beryl. Na2SiF6 requirements to form water-soluble salts of beryllium were determined for three different samples--two clayey ores containing 0.6 and 1.3 pct BeO, respectively, and a calcareous ore containing 0.6 pct BeO. The ores were sintered with Na2SiF6 at 750° C for 3 hours. About 80 pct of the beryllium was rendered water soluble by sintering the 0.6-pct BeO ores with 30 and 40 lb Na2SiF6 per lb BeO contained in clayey and calcareous ores, respectively. The higher grade 1.3-pct BeO clayey ore required only 20 lb Na2SiF6 per lb BeO to solubilize over 80 pet of the beryllium. As the 0.6-pct BeO clayey ore was possibly the most representative of the deposit as presently delineated, leach liquor prepared from this sample was treated to recover beryllium salts. About 60 pet of the beryllium contained in the ore was recovered as beryllium hydroxide, which then was calcined to yield a 99-pct BeO final product by means of the following operations: (1) Sintering with Na2SiF2, (2) leaching with water, (3) precipitating crude Be(OH)2 by adding NaOH, (4) filtering to separate the hydroxide from the NaF solution, (5) redissolving the crude Be(OH)2 in excess NaOH, (6) filtering to reject caustic-insoluble impurities, and finally (7) boiling the Na2BeO2 filtrate from (8) to precipitate pure Be(OH)2. Reagent consumption was 49 lb Na2SiF6 per lb BeO recovered and 17 lb NaOH per lb BeO.

Jan 1, 1963

By A. R. Taylor

Low-temperature heat capacities of cesium chloride (7° - 300° K) and cesium iodide (13° - 300°K) were measured with an adiabatic calorimeter. The heat-capacity measurements were analyzed graphically to determine smooth values of heat capacity, entropy, enthalpy function, and free-energy function at 10° K intervals and at 273.15° and 298.15° K.

Jan 1, 1963

By P. T. Brooks

The selective recovery of nickel and cobalt from impure raw materials is being investigated by the Bureau of Mines as part of a program to develop improved procedures for preparation of pure metals. A combination solvent extraction-electrolytic process has been developed in the laboratory that enables preparation of high-quality nickel and cobalt from nickel oxide containing, in percent, 76 nickel, 0.8 cobalt, 0.5 magnesium, 0.2 iron, and lesser quantities of copper, zinc, and other metals. The oxide was smelted, using carbon as reductant, and cast into anodes. These anodes subsequently were dissolved in diaphragm-type electrolytic cells. Nickel and cobalt were deposited separately from appropriate electrolytes, concurrent with dissolution of the impure anodes. Anolyte containing nickel and cobalt in the form of chlorides and sulfates was treated for removal of impurities and separation of nickel and cobalt. First, iron and aluminum were removed as hydroxides by adding nickel hydroxide to raise the pH of the anolyte from 2.3 to 4.5. Next, the pH was adjusted to 2 by adding hydrochloric acid, and the solution was treated by solvent extraction to separate nickel and cobalt.

Jan 1, 1963

By Charles Prasky

This report describes and appraises recent progress in the development of a differential sulfatizing process for recovering a ferrograde manganese oxide from low-grade manganiferous ferruginous materials in the Cuyuna range. Individual process steps were carried out successfully using a 20-inch-diameter shaft for continuous countercurrent sulfatization of the manganese, a multiple-compartment rotary drum for leaching the water-soluble manganese sulfate, a submerged-combustion evaporator for the recovery of monohydrate crystals of manganese sulfate, and a shaft furnace for the thermal decomposition of sulfate crystals for production of a ferrograde manganese oxide and a sulfur dioxide gas suitable for sulfatization of fresh are. Of the two general kinds of Cuyuna manganiferous materials--the carbonate slates and the oxidized ores--only the slates were studied at pilot scale.

Jan 1, 1963

By M. M. Wong

Electrolysis of titanium carbide and a material consisting of titanium, carbon, nitrogen, and oxygen as soluble anodes in Used electrolytes was investigated by the Bureau of Mines for the preparation of crude titanium metal. Tests made in all-chloride electrolytes showed only a low recovery of titanium as well as a substantial volatilization of titanium trichloride (TiC13) when present in the electrolyte. Electrolysis at 750° to 850° C in a mixture containing 85 percent NaC1-15 percent potassium floutitanate (K2TiF6) yielded as high as 91 percent recovery of titanium from titanium carbide and 62 percent recovery of titanium from the titanium-carbon-nitrogen-oxygen material. Problems associated with the preparation of crude metal by fused-salt electrolysis are discussed. The crude metals produced from both anode materials were electrorefined in a sodium chloride-titanium chloride (NaCl-TiC12) electrolyte, and ductile titanium metal was obtained.

Jan 1, 1963

By T. A. Henrie

A technique was devised for measuring the rate of chemical reactions between reactive metals and molten-salt mixtures at high temperatures. The rate of the heterogeneous reaction between high-purity titanium metal and titanium trichloride in molten sodium chloride was determined. The reaction is surface-controlled, and the heat of activation is 8.29 kilocalories per mole TiC13. An active site or reaction nuclei is created by adsorbing a TiC13 molecule at the metal surface. Reaction of the second TiC13 species forms an activated complex that decomposes into three TiC12 molecules.

Jan 1, 1963