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By C. H. Riggs

This report describes the geology and reviews the oil-production history of the Dutcher sands of Pennsylvania age in the Muskogee oilfield. The geology and production history are presented not alone as a review of the past behavior of the field but also to interpret the possibilities for future production of oil from semidepleted sands in this and similar areas. The Muskogee field, one of the oldest oil-producing areas in Oklahoma, yields paraffin-base oil of 40° API gravity -a gravity higher than that of most Oklahoma oils. Oil was discovered in the townsite of Muskogee in 1894 but was not produced in commercial quantities until 1904. A peak yearly rate of 1,340,000 barrels of oil was attained in 1910 (see table 1).

Jan 1, 1959

By Leonard F. Heising

Domestic production of Metallurgical-grade manganese has contributed such a small percentage of the United States industrial demands that areas known to contain large tonnages of low-grade manganese ore have been investigated by the Bureau of Mines to reduce this country's dependence on foreign ores. A major source of low-grade manganese is the Cuyuna iron range in Minnesota. The entire Cuyuna iron range is covered by an overburden of glacial drift that, in some places, reaches depths of 200 feet or more. Prospecting and exploration must be guided by geophysical methods, drilling results, or projections of exposures found in operating mines because there are no outcrops near the productive parts of the range. Past drilling for the purpose of outlining iron ore generally was confined to the highly oxidized zones. Much of the manganese with which the Bureau of Mines is concerned occurs in thin-bedded unoxidized iron formations, too low in iron content to have been of interest to those seeking commercial iron ore. The primary objective of the core-drilling reported here was to obtain cores of different classes of manganiferous rocks and to determine whether or not the samples were amenable to beneficiation.

Jan 1, 1959

By David J. Kusler

This report describes a primary or direct, continuously sampling, and automatically averaging gravimetric method for analyzing gaseous mixtures of carbon dioxide, carbon monoxide) hydrogen, and (by volume measurement) nitrogen. The gaseous mixture is analyzed by passing it at a controlled and definite rate through a system that permits carbon dioxide and water retained by appropriate absorbents to be determined and the residual-gas volume (essentially nitrogen) to be measured. The accuracy and dependability have been established by comparison with very carefully conducted Orsat analyses. The method was developed for, and has been satisfactorily applied to, the analysis of blast-furnace top gas. It permits relatively attention free operation, using simple and low-cost materials usually found as basic equipment in the analytical laboratory. It provides, over a wide range of time or sampling intervals (from less than 1 to over 24 hours), the average composition, in terms of volume-percent, for those components usually determined in blast-furnace gas, if (as is usual) the flow rate of gas from the blast furnace is essentially constant over a selected analysis interval. Oxygen and methane are not determined; but, since these gases are normally absent or present only in traces, their analysis is seldom required.

Jan 1, 1959

By B. C. Parks

This paper is a report on the relationships between petrographic composition, chemical composition, physical properties, and thermal behavior of banded bituminous coal. It describes the relationships between petrographic composition, behavior in various laboratory tests, and carbonizing properties of different petrographic types of coal that occur in relatively thick benches in a single bed of high-volatile A bituminous coal - the Hernshaw bed of Boone County, W. Va. Thin-section microscopic analysis and free-swelling index determinations of the thin-section samples were made of a standard column sample. A standard face sample, a representative channel sample, and representative samples of two prominent petrographic benches of bright and dull coal were subjected to chemical analyses and free-swelling-index, plasticity, dilation, agglutinating, low-temperature carbonization, and BM-AGA retort tests. A float-and-sink separation was also made of part of the standard face sample. The fractions from this gravity separation were subjected to petrographic and chemical analysis and free-swelling-index, plasticity, and dilatation tests.

Jan 1, 1959

By L. Allan White

Instrumental analysis is an indispensable tool to many phases of research on rare-earth metals and their compounds; therefore, the development of new and improved instrumental techniques is essential. This report describes an emission spectrometric analytical method using direct-current carbon-arc excitation of various rare-earth-oxide mixtures. Lanthanum oxide serves the dual purpose of an internal standard and a constant major constituent. The versatility of the method was demonstrated by three different applications: (a) Analysis of complex rare-earth concentrates; (b) determination of impurities in high-purity rare-earth oxides; and (c) detection of rare-earth elements in other types of matrices, such as those resulting from beneficiation of rare-earth ores. The average error of analysis in the concentration range of 0.2 to 10.0 percent was 14.6 percent for a group of complex synthetic mixtures of rare-earth oxides. An average error of analysis in the concentration range of 0.05 to 0.50 percent was 21 percent for a group of high-purity rare-earth oxides.

Jan 1, 1959

By D. E. Wolfson

This report describes the carbonizing properties of the principal coal beds of Allegheny County, Pa., which rank low in the high-volatile A bituminous classification. Seven coal samples from 3 coal beds were selected for study, as follows: 2 each from the Redstone and Pittsburgh beds and 3 from the Upper Freeport bed. Selection was based on estimated reserves. The samples of Upper Freeport and Pittsburgh coals were satisfactory chemically for producing metallurgical coke. The ash contents of the samples of Redstone coal were moderately high. One of the samples of Redstone coal was high in sulfur content, and it would be difficult to upgrade to meet present metallurgical standards.

Jan 1, 1959

By J. J. Demeter

As part of its work on converting coal to fluid fuels, the Federal Bureau of Mines has been studying the synthesis of liquid fuels from carbon monoxide and hydrogen by Fischer-Tropsch synthesis. A fluidized bed of nitrided, fused-iron catalyst has been operated successfully to produce high yields of oxygenated compounds. Trouble-free operation continued for over 800 hours, and the test was terminated voluntarily. About 85 percent of the fresh feed was converted when the unit was operated at a space velocity of 500 hr.-1, a 12:1 recycle-to-fresh-feed-gas ratio, a 300-p. s. i. g. pressure, and a temperature of 252° C. When operating at a fresh-feed-gas space velocity of 1,000 hr.-l and a 9:1 ratio of recycle to fresh gas, conversion of fresh feed was 68 percent, and the product yield was 235.9 grams per cubic meter of synthesis gas converted. The oxygenate and C5 and heavier hydrocarbon yield was 110.6 grams per cubic meter of gas converted, 83 percent of this was oxygenates. The atom ratio of N:Fe of the catalyst, initially 0.455, decreased to 0.288 by the end of the 800-hour experiment. Nevertheless, the yield of oxygenated compounds per cubic meter of H2 + CO converted at the end of the run was approximately the same as that obtained 500 hours earlier with identical operating conditions. X-ray analysis of the discharged catalyst indicated that only ?-iron carbonitride was present. Sieve analysis of the discharged catalyst indicated that only 2 percent of fines was produced during the reduction, nitriding, and synthesis.

Jan 1, 1959

By Arnold B. Hubbard

This report presents a hydrogenolysis study undertaken to obtain information on the constitution of the kerogen or organic material in Colorado oil shale and to determine some of the properties of the hydrogenolysis products. The high yield of hydrogenolysis products was separated, so far as possible, into type compounds; a number were identified. The results thus obtained were used as a basis for proposing the possible existence of certain structures in kerogen. To the authors' knowledge, few or no hydrogenolysis studies have been made of Colorado oil-shale kerogen by others. However, this method has been used in studying the constitution of coal. In general, the coal studies involved treating pulverized coal at different temperatures and hydrogen pressures with different catalysts. In some instances different solvents were used during the treatments.

Jan 1, 1959

By W. M. Mahan

This report describes work carried out by the Federal Bureau of Mines in cooperation with the General Services Administration (GSA). Tests on nickel oxide reduction were conducted at the Pyrometallurgical Laboratory at Pitts-burgh and Bruceton, Pa., and at a rented plant at Canonsburg, Pa. Nickel oxide was reduced to sponge nickel, which was then melted to produce specification-grade nickel ingots containing a minimum of 98.50 percent nickel plus cobalt and a maximum of 1.00 percent cobalt. One purpose of this study was to determine if specification-grade nickel could be made from nickel oxide produced at the United States-Government-owned plant at Nicaro, Cuba, in pilot-plant scale operations involving direct reduction and melting processes. A second and equally important purpose was to obtain cost data on the pilot-plant operation to estimate the cost of producing ingot nickel at an annual rate of 12 million pounds. Laboratory tests verified that nickel oxide, in saggers and in the presence of anthracite fines and dolomite in the ratio of approximately 20:5:1, could be converted to sponge nickel when heated to approximately 1,900° F. for about 2 to 4 hours, depending on the size and density of the oxide charge. The tests also determined the type of saggers suitable for pilot-plant operations.

Jan 1, 1959

By R. Barany

This paper reports determinations of heats of formation (from the oxides and elements) of crystalline cadmium metasilicate and crystalline lead meta-silicate by hydrofluoric acid solution calorimetry. The results, in conjunction with known entropy values, yield free energies of formation. There are no earlier data of this type for cadmium metasilicate. The results of this investigation for lead metasilicate deviate from the literature values (which are less reliable) in the direction of increased thermodynamic stability. Both cadmium and lead metasilicate are much less thermodynamically stable with respect to their constituent oxides than are the corresponding compounds of the alkaline earth metals.

Jan 1, 1959

By R. L. Montgomery

The literature has been surveyed and values recalculated for the heats and free energies of formation of solid rare-earth compounds at 298° K. In most instances it was necessary to estimate the entropies. Thermodynamic properties of aqueous rare-earth ions have also been calculated. INTRODUCTION The accumulation of thermochemical data on rare-earth compounds in recent years makes it possible to review the subject and to obtain more consistent and more reliable information than was available previously.

Jan 1, 1959

By Van E. Shaw

Bastnaesite is a natural rare-earth fluorcarbonate of the cerium group that affords an abundant and high-grade source of the lighter rare-earth elements. A simple and efficient method has been developed by the Bureau of Mines for extracting rare-earth compounds from this mineral. Digesting of a flotation concentrate with sulfuric acid converts the rare-earth compounds from fluorcarbonates to sulfates. Action of the acid releases gaseous com-pounds of fluorine and silicon, leaving the sulfated material free of these elements; carbon dioxide from carbonate decomposition is eliminated at the same time. Calcining the sulfated material at 1,200° F. renders the gangue constituents insoluble, whereas the rare-earth sulfates are left in water-soluble form. Leaching with water yields a solution of pure rare-earth sulfates. Bastnaesite could become prominent as a source of cerium-group rare-earth elements. It is rich in the light rare-earth elements and comparatively easy to process; reserves of the mineral are extensive enough to supply a greatly expanded market for many years.

Jan 1, 1959

By H. S. Caldwell

A magnesium-base incendiary alloy, containing about 20 percent cadmium, 4 percent aluminum, and 0.5 percent zinc, was investigated in a series of vacuum-distillation experiments to determine the feasibility of recovering magnesium and cadmium as refined metals. Alloys prepared in the laboratory and actual bomb-casing alloy were studied at temperatures of 550° to 750° C. and pressures of 100 to 150 microns. Simple distillation and fractional distillation methods were only partly effective in separating the cadmium and magnesium. They were separated satisfactorily, however, with a special vapor baffle designed to condense the metals selectively. Magnesium and cadmium products were 99 percent pure and together comprised 82 percent of the total condensate. About 17 percent of the condensate was intermediate-grade alloy that could be recycled with new charge and contained about 70 percent magnesium and 30 percent cadmium.

Jan 1, 1959

By Alton B. Cook

Equipment has been designed and fabricated for study of the vaporization of oil during gas-cycling operations, A sand-packed steel tube, which can be rotated to minimize gravity drainage, is used as a model oil reservoir. A minute windowed cell at the discharge end of the tube through which the liquid-gas interface may be observed, makes possible the separate removal of produced free gas and gas-saturated oil. The operation of the model oil reservoir, and auxiliary equipment, are described by use of a schmatic flow diagram. Details of the specially designed equipment are illustrated by isometric and pictorial drawings, and a description of the experimental procedure is given.

Jan 1, 1959

By E. G. King

Cerium and thorium sulfides have found use as crucible materials for melting certain radioactive metals. However, thermodynamic treatment of these sulfides has been hampered by lack of experimentally derived entropy values. This Bureau of Mines report describes heat-capacity measurements between 51° and 298° K, and entropy evaluations at 298.15° K, for cerium monosulfide (CeS), cerium sesquisulfide (Ce2S3), and thorium disulfide (THS2). The entropy values, with Literature results for the heats of formation, are used to obtain free energies of formation at 298.15°K. MATERIALS The samples used in this work were supplied by Prof, Leo Brewer of the Department of Chemistry, University of California. The methods of preparation and some of the physical and chemical properties of these sulfides were given by Eastman and coworkers.3 4/ Chemical analyses, conducted in our laboratory, gave the following results:

Jan 1, 1959

By R. L. Grant

An investigation was undertaken by the Bureau of Mines to determine the relationship between freespace and ignition probability for borehole shots. A series of experiments was concluded which covered six freespace conditions for a pemissible explosive in a 3/4-inch borehole and encompassed some 700 shots. The results were analyzed statistically. From the analysis of variance, it was concluded that the freespace means were different and that this conclusion is not impaired by possible differences in the explosives used. Within the limitation of this experiment, a definite relationship was found between the freespace and the ignition probability. Specifically, the incendivity increases with increased freespace up to a maximum; beyond this maximum there is some indication of decreasing incendivity. Further investigations are in progress to establish whether the effects of freespace on ignition probability reported here are applicable to the large test gallery, INTRODUCTION A borehole loaded with an explosive charge is a common feature of the routine gallery tests for determining the permissibility of coal-mine explosives, of Experimental Coal-Mine shots, and of the small steel cannon shots used in connection with certain research programs on the ignition of firedamp (6, 10).6/ The question of the interrelationship of freespace, weight of charge, and ignition probability of the methane-air atmosphere has been raised

Jan 1, 1959

By K. K. Kelly

METALLURGICAL thermochemistry of titanium is a broad subject and (if data were available) could include a wide variety of topics. The present report is restricted to extractive metallurgy and to substances and reactions that bear upon the magnesium, sodium, and hydrogen-reduction processes employing titanium tetrachloride. The aim has been to present enough data so that the reader not only can check: the calculations for the reactions discussed but also can conduct related calculations if he so desires, without recourse to other compilations of data. The subject matter divides naturally into two parts-the selection of the data to be adopted and the application of these data to pertinent metallurgical reactions.

Jan 1, 1959

The complex organic chemicals in coal differ from those in petroleum mainly by the ratio of carbon atoms to hydrogen atoms; this ratio is about 2 for coal and 1 for petroleum. By changing the ratio, coal can be converted into compounds similar to those found in petroleum. In. very simplified form, omitting here the special conditions required, the paths by which this can be done are: [ ] Part or all of the coal is first gasified by reaction with steam and oxygen, either in a gasifier or while the coal is still in place underground. The resulting gas is mainly hydrogen and carbon monoxide, with impurities that .must be removed before further processing by one of the following routes.

Jan 1, 1959

By Victor Kalcevic

A gas-flow retort for thermal processing of oil shale to recover shale oil was developed by the Bureau of Mines at its Oil-Shale Demonstration Plant, Rifle, Colo., from 1948 to 1952. The retort is a crossflow gas-to-broken-solids heat exchanger. The heating medium is the gas produced in the shale retorting process. The gas is heated in specially designed stoves outside the retort and recycled to the retort. Oil shale from the Mahogany ledge section of the Green River formation in northwestern Colorado was the material processed. Indicated maximum oil recoveries for 20-to 25-gallon-per-ton shale in a l2-inch-thick shale bed and a 20-inch bed are 96 and 91 weight-percent of Fischer assay, respectively. Heat requirements for maximum recovery are 600 to 750 B.t.u. per pound of shale. Properties of the recovered shale oil are affected slightly by shale-bed thickness and extent of retorting. Oil recovery from oil shales assaying over 30 gallons per ton is lower than that from leaner shales.

Jan 1, 1959

By Thomas C. Atchison

The purpose of this Bureau of Mines investigation was to measure the amplitude and shape of the strain pulse and the size of the crushed zone produced in a granite by different explosives and to determine how these quantities are related to the detonation properties of the explosives. The reflection theory of rock breakage has shown that the amplitude and shape of the strain pulse incident at a free surface determine the fragmentation and volume of rock broken. Determination of the properties of an explosive that control the characteristics of the strain pulse produced in the rock will help in evaluating explosives for use in blasting. The investigation showed the different explosives produced a twofold variation in the amplitude of the strain pulse but little variation in the shape of the pulse. The explosives also produced a twofold variation in the volume of the crushed zone, but differences among the explosives were more accurately determined by strain-amplitude measurements than by crushed-zone measurements. The peak amplitude of the strain pulse and the volume of the crushed zone correlated with the calculated detonation pressure of the explosive.

Jan 1, 1959