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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 H. G. Wolfhard

The propagation of explosions through short cylindrical channels has been investigated by the Bureau of Mines. In the experimental apparatus set up by the Bureau, a single such channel formed a connection between a small explosion vessel in which a gaseous explosion was initiated and a larger, partly enclosing, explosion vessel filled with suitable gaseous mixtures; the larger vessel permitted observation to determine if an explosion was induced therein by mass, energy, and species transfer through the channel, as a result of tie initial explosion, It has been found that transmission of flame through to channel is not an essential to induce the second explosion, for hot gases from an extinguished explosion are able to ignite cold combustible mixtures in the larger vessel. The schlieren patterns of flames or hot burned gases emerging from a channel into the explosion chamber were photographed. These show, in most instances, that vortexes of hot gas ejected from the jet into the cold explosive mixture are responsible for ignition. The study has practical significance in problems of rendering electrical equipment safe for use in potentially flammable atmospheres, INTRODUCTION The propagation of flames through cylindrical or annular channels has practical importance in flameproofing electrical equipment and for flame traps. Much practical work has been done to determine the minimum safe breadth of flanges and the maximum safe gap between the flanges that will permit venting an electric motor without allowing flames to pass.

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 K. K. Kershner

The purpose of this investigation was to develop methods, on a laboratory scale, for recovering tin from Bolivian metallurgical slimes. Petrographic and chemical analyses were made of slime ore fractions from several well-known tin operations. High percentages of the total tin were volatilized as chlorides at temperatures below 600° C. Under optimum conditions reaction rates were relatively rapid, and the chloridizing reaction approached completion. Owing to the low temperatures involved and the high yields of tin, the process was considered to have possibilities for treating Bolivian slimes on a commercial basis. ACKNOWLEDGMENTS Appreciation is hereby extended to the Patino Mines and Enterprises, Inc., of Bolivia, for supplying slimed tin ores that were used in the experimental work. This company has since been nationalized.

Jan 1, 1959

By Kenneth Lipman

Auxiliary equipment was assembled around a purchased oscillograph to permit observation of the current and voltage characteristics of low-energy, capacitance-discharge sparks having durations of at least 10 mµ-sec. Circuit details of the assembled apparatus, performance characteristics of the complete system, and some preliminary data from representative self-initiated sparks are given in this report. INTRODUCTION One of the subjects of continuing research by the Federal Bureau of Mines Division of Explosives Technology is the ignition of explosive-gas mixtures by means of low-energy capacitance sparks. Quite early in these investigations it was recognized that understanding the gas-ignition phenomena would be facilitated by detailed information about the performance of the ignition source (spark) under the actual conditions of interest; however, the sparks of practical interest are nonrepetitive transient phenomena whose duration could reasonably be estimated to be in the time range of 1 mµsec. to 1 µsec. As such, the only feasible method of obtaining detailed information was and is oscillographic representation of the pertinent current and voltage transients. It was not until 1947 that a suitable, commercial, dual-channel oscillograph could be obtained as the basic instrument for these studies; the instrument specified in 1947 was delivered in 1950. This paper describes the auxiliary

Jan 1, 1959

By E. L. Litchfield

Spark ignition of combustible-gas mixtures is a relatively old subject of investigation and has been treated both experimentally and analytically by many people. Elements of static and current electricity are almost always present in mining and industrial operations, and the spark can be an extremely efficient source of ignition. Thus the practical interest of such problems as the "intrinsic safety" of electrical apparatus is obvious. Ignition and quenching phenomena are the primary laboratory representatives of combustion phenomena that are dynamically nonsteady, and such nonsteady phenomena playa considerable part both in industrial processes and in safety matters, although they are of less immediate practical interest. Considerable effort has been expended by the Federal Bureau of Mines in investigations of spark ignition.5 6 7 8/ Primarily, this work has established the significance of several of the parameters involved. Although the

Jan 1, 1959

By W. W. Agey

Under terms of cooperative agreements, the Federal Bureau of Mines Inter-mountain Experiment Station assisted the General Services Administration (GSA) in operating the manganese-ore purchasing depots at Deming. N. Mex., and Wenden, Ariz. A resident metallurgist stationed at the depots directed sampling of the ore lots for assaying, took samples for amenability testing, calculated acceptances for payments to shippers, and served as technical adviser to the depot manager. The Intermountain Experiment Station at Salt Lake City, Utah, tested the amenability of the ores to determine how much of the manganese could be recovered in concentrates assaying a minimum of 40 percent manganese (Mn) and containing a maximum of 16 percent iron (Fe), 15 percent silica (Si02) plus alumina (AI203), 0.3 percent phosphorus (P), and I percent copper (Cu) plus lead (Pb) plus zinc (Zn). All chemical analyses of the ores and test products were done at Salt Lake City. In all, 567 ore lots submitted to the Deming depot were tested by flotation to determine their amenability to concentration into specification-grade material; 421 lots were amenable, and 146 were unamenable, primarily because of high copper content or excessive silica or iron in the flotation concentrate. Chemical analyses totaling 42,700 were made on the ores submitted to the Deming depot and on the products of the amenability-test program.

Jan 1, 1959

By N. E. Hanna

The effect of small percentages of sodium chloride on the incendivity of permissible explosives was studied by the Bruceton up-and-down technique in gallery tests. Both the reduction in incendivity achieved by addition of sodium chloride and application of the test method to explosives evaluation are discussed. It is demonstrated that the up-and-down technique in gallery testing is suitable for distinguishing differences in incendivity between different explosive compositions and between lots of the same composition. The study also shows that addition of relatively small quantities of sodium chloride tends to reduce the incendivity of explosives to firedamp, but addition of sodium chloride cannot insure reduced incendivity. Any improvement attributable to the salt can be counteracted by undefined variations in the explosive. The need for experimental investigations of a number of factors that may affect the safety of permissible explosives is emphasized. ACKNOWLEDGMENTS Grateful acknowledgment is made of the assistance of Roy L. Grant in analyzing for normality of distribution of the data obtained by the up-and-down methods and to Harold E. Tubbs for numerous calculations.

Jan 1, 1959

By J. B. Gayle

The Bureau of Mines sole-heated oven has been used for studying coal expansion for some 20 years. During the period before 1940 emphasis was placed on studies of the mechanism of coal expansion and the effects of variations in operating conditions on the results. Since 1940 emphasis has shifted to a survey of the expansion properties of various coking coals. Because additional information concerning a number of unsolved problems in connection with the earlier studies appeared highly desirable, this investigation of the use of sole-heated ovens for studying coal expansion was undertaken. The principal findings, in order of their discussion in the text, may be summarized as follows. 1. Expansion results for binary blends of coking coals exhibit nonadditive behavior, both positive and negative deviations from additive behavior being noted, depending on the particular coals tested. Additive behavior can be achieved, however, either by charging the blend components in separate layers (which indicates that the observed phenomena are not characteristic of the particular expansion oven used) or by testing relatively coarse sizes of coal (which suggests that the effects of crushing on the expansion properties of coking coals may be even more complex than is generally recognized).

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 J. G. Walters

In a survey of the coking properties of United States coals, the Bureau of Mines has accumulated data on more than 500 coals and blends tested by the Bureau of Mines-American Gas Association (BM-AGA) method.4/ The importance of these tests depends upon the fact that a greater number of different coals has been tested in this apparatus than in any other of similar scale, thus permitting comparison of the carbonizing properties of many coals. Evaluation of BM-AGA results with respect to industrial data supplied by member firms of the American Gas Association was one of the first objectives in developing this test apparatus and procedure. Early data showed that, de-pendent upon BM-AGA carbonizing temperature, BM-AGA and commercial results agree closely.5/ Because of limited data, statistical relationships were not established at that time.

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 J. H. Field

Capital and operating costs have been estimated for removing sulfur dioxide from flue gases of a powerplant of 12,000-kw. capacity by liquid-purification processes, using limestone, ammonia, or sodium sulfite as the reactant. The annnonia and sodium sulfite processes yield end products that may be marketable. Coals containing about 1.5 and 5.0 percent sulfure have been considered. The sulfur dioxide content of the gases to be treated is 0.083 and 0.30 percent, respectively. Estimates have been made for 90-percent removal of the sulfur dioxide from both gases. A third instance has been considered in which 70 percent of the sulfur dioxide is removed from the flue gas of 0.30-percent concentration. The scrubbed gas would contain 0.09 percent sulfur dioxide, which might be within the permissible limit for discharge to the atmosphere in most areas. Although it is unlikely that flue gases with sulfur dioxide concentrations of less than 0.10 percent would require purification, a cost estimate for such a gas is included because an estimate is available for a British plant employing the limestone process at these conditions. Capital investment and operating costs, with no credit for products, are lowest for the limestone process for gases of both concentrations. Crediting the ammonium sulfate and sulfur produced in the ammonia process at their market prices at the end of 1956 of $32 and $28 per ton, respectively, the operating costs of the ammonia process become the lowest for purification of the gas containing 0.30 percent sulfur dioxide. The operating costs of the sodium sulfite process for purifying gas of high sulfur dioxide content approach those of the limestone process when the byproduct sulfur dioxide is credited at $14 per ton. Even if credit for products is allowed for the ammonia and sodium sulfite processes, the operating costs are higher than those of the limestone process for the gas of low sulfur dioxide content. Because of the large quantity of materials that would be produced by removing sulfur dioxide from a relatively small number of plants, credit for products should be allowed with extreme caution.

Jan 1, 1959

By E. C. Tarpley

An acid-extraction procedure developed in Germany for determining mineral matter in coal was investigated by the Bureau of Mines to determine its application to American coals. It was found to be suitable for all ranks of coal from anthracite to lignite if modified slightly for coals containing considerable quantities of calcium compounds, such as calcite or calcium humate. The precision of the method is satisfactory, and the results are probably closer to the true content of mineral matter than those obtained by empirical formulas. The method requires considerably more analytical data than the Parr or approximation formulas but is no more time consuming than obtaining the necessary data for the King, Maries, and Crossley formula (theoretically the most comprehensive empirical formula used). An appendix to this report includes a detailed description of a recommended procedure.

Jan 1, 1959

By J. F. Barkley

Field tests were made on the rate of corrosion of 30 materials used in air preheaters under regular operating conditions, and the buildup of deposits was observed. Twenty-three materials were tested with coal as the fuel on an underfeed stoker and seven with oil, including a short period with pulverized coal as fuel, The plant equipment is described, and pertinent plant operating data are tabulated. Figures 17 and 19 (pp. 24 and 27) give the results of corrosion tests on the uncoated metal test specimens. The information obtained from these tests follows the general pattern described in Bureau of Mines Report of Investigations 4996, Corrosion and Deposits in Regenerative Air Preheaters. The deposits were similar, and the corrosion rates of Cor-Ten and Mayari-R steel (previously found to be essentially the same at the Harding Street Station using coal) continued to show little difference at the Marion Generating Station using principally oil. The one high-alloy steel tested, type 321, showed a much higher corrosion rate than the low-alloy steel, Cor-Ten.

Jan 1, 1959