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By D. F. Walsh

A study of damping capacity was made on a number of magnesium-base alloys, commercial types and experimental compositions. Hardness and tensile properties were determined, and the microstructure of each alloy was examined. Alloys of low yield strength, in general, possessed high damping ability. A correlation was established between damping capacity and composition.

Jan 1, 1962

By L. F. Willmott

Pulverized high-volatile A bituminous coal was gasified with oxygen and superheated steam in a pressure-gasification pilot plant equipped for slurry feeding. The minimum ratio of water to pulverized coal that could be pumped satisfactorily as a slurry was about 1 to 1. Heating this slurry produced a suspension of coal in superheated steam having a steam-to-coal ratio greater than the 0.3 to 1 proportion that is considered optimum for pressure gasification of pulverized coal. A steam separator removed enough steam to provide ratios down to about 0.5 to 1, but a 0.3 to 1 ratio was not achieved. Gasification of Sewickley coal produced a synthesis gas containing about 36 percent H2, 46 percent CO, and 13 percent CO2, Gas output, gas composition, and coal and oxygen requirements were Virtually the same as for a pilot plant equipped for fluidized-coal feeding. Typical results from the slurry-fed plant at 300 psig were carbon gasified, 95 percent; coal requirement, 34 lb/M (thousand) std cu ft CO + H2 produced; oxygen requirement, 365 std cu ft/M std cu ft CO + H2 produced. The results showed that the two feeding methods are equally satisfactory from the standpoint of gasification. A choice between a fluidized-coal gasification process or a slurry gasification process depends on considerations relating to the coal-feeding phase itself, including capital and operating costs, manpower requirements, safety, and flexibility of operation.

Jan 1, 1962

By F. B. Petermann

The Bureau of Mines conducted electric furnace smelting tests on sintered flotation concentrate and siliceous log-washed are. The flotation concentrate was derived from the Maggie Canyon deposit of the Artillery Mountains area, Mohave County, Ariz., and contained, before sintering, 35.6 percent Mil and 19.4 percent Si02 + A1203. The log-washed ore was from the McGregor deposit of the Artillery Mountains area, Mohave County, Ariz., and contained 31.2 to 33.6 percent Mil, 19.5 to 27.6 percent Si02 + A1203, and 2.5 percent Pb. This work was undertaken to determine the most effective smelting technique for producing standard products from such nonspecification ore and concentrates. The objective was to collect data, using a small furnace, which would be reasonably accurate and permit extrapolation to large-scale practice for comparing with results on specification-grade are.

Jan 1, 1962

By G. V. Sullivan

This report summarizes the results of a preliminary study concerning manganese extraction from low-grade dolomitic materials from the Philipsburg district in Montana by the Dean-Leute ammonium carbamate process. Studies were made to determine the relationship between the variables involved in treating these materials by a roast-leach process and the amount of manganese extracted. The variables studied were the roast temperature, the roast particle size, the molar ratio of NH3 to CO2 in the leach solution, the liquid-solid ratio in leaching, the leach time, and the size of the particles being leached. The roast-leach studies were statistically designed, and the experimental results were evaluated by an analysis of variance.

Jan 1, 1962

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 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 John Fitzpatrick

In this Bureau of Mines investigation a device was developed that permits the determination of the modulus of elasticity of the stress-relief cores obtained in the process of making in situ stress measurements. This determination is made by hydraulically loading the external surface of the stress-relief cores and by measuring the corresponding borehole deformation. The theoretical relationship between the borehole deformation, the applied pressure, and the modulus of elasticity is presented. Also, experimental results obtained from measurements on a simulated stress-relief core made of aluminum and on a limestone stress-relief core are given. Because of the symmetrical loading obtained with this device, the isotropy of the core material can be evaluated. With this device it is also possible to study the effect of eccentricity, that is, the effect within cores in which the inner hole is not coincident with the long axis of the specimen.

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

By W. W. Weller

This report provides low-temperature heat-capacity data and entropies at 298.15° K. for magnesium metavanadate (MgV206) and magnesium pyrovanadate (Mg2V207). The work completes low-temperature measurements planned for alkaline-earth vanadates; an earlier report dealt with calcium vanadates.4 No similar data for these compounds have been published previously. Free energy of formation values at 298.15° K. were derived by combination of the present entropy values with heat of formation data. MATERIALS The materials used in the measurements were portions of the samples described in a previous Bureau of Mines publication by King, Koehler and Adami.5 Methods of preparation, chemical analyses, and X-ray examinations are covered in this paper. The indicated purity of the samples was 99.9 pct.

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 H. E. Powell

Because of increasing consumption of high-and super-duty refractories, the Bureau is studying the feasibility of beneficiating submarginal and marginal clays. Diverse mineral dressing tests were used to beneficiate samples from the east-central Missouri fire clay district. Standard ASTM tests were used to determine refractory properties of both crude and beneficiated clay samples. Marginal and submarginal clays containing impurities were effectively beneficiated by both wet-cyclone and wet-table treatment, but the wet-cyclone treatment was cheaper. Ion-exchange resins in the hydrogen form will probably prove more effective in removing potassium, the only alkali in Missouri fire clays to be a problem. Resins with greater cross linkage are more effective than resins with less. Roasting the crude clays before removing alkalis by chemical leaching was ineffective. By applying ultrasonic energy at a frequency of 10 to 25 kilocycles to aqueous suspensions of the clays, subsequent ion-exchange extraction of potassium was slightly improved. Higher frequency ranges did not help.

Jan 1, 1963

By R. Barany

The heats of formation at 298.15° K of calcium tungstate, calcium molybdate, and magnesium molybdate were determined by solution calorimetry. For the heats of formation from the elements, the values obtained were calcium tungstate, -402.4 ± 0.5 kcal/mole, calcium molybdate, -369.5 ± 0.3 kcal/mole, -334.8 ± 0.2 kcal/mole. For the heats of formation from the oxides J the values obtained were calcium tungstate, -49.2 ± 0.4 kcal/mole, calcium molybdate, -39.6 ± 0.1 kcal/mole, and magnesium molybdate, -12.9 [ ] 0.1 kcal/mole.

Jan 1, 1962

By R. F. Tenney

No detailed information has been published heretofore on the performance of small industrial-type anthracite stokers in building-heating service, apparently because of the difficulty of comparing the performance of one unit with that of another over an entire season's operation. Studies of competitive heating fuels have been similarly handicapped, and attempts to compare fuels are seldom technically sound in this investigation, the performance of a 60-in. Losch4 stoker burning rice-size anthracite in a standard commercial boiler was observed during a 4-month winter-spring season. It was used to heat two buildings at the Bureau of Mines' Anthracite Research Center at Schuylkill Haven, Pa., with the customary type of automatic pressure-range control. Attendance was limited to inspecting, fuel weighing, data recording, and ash removal. Results were computed daily and grouped by weekly periods to minimize daily irregularities. The same stoker-boiler unit had already been tested in a series of American Society of Mechanical Engineers (ASME) test code runs, with the stoker running continuously and with other conditions well stabilized A comparison of results from the code test and the building-heating tests provided information not available in the past for a single stoker unit, assisted in analyzing heat losses not computable in a cyclic operation, and established a basis for evaluating stoker performance in heating service.

Jan 1, 1963

By R. L. Montgomery

Heats of solution of cerium metal and cerium (III) chloride in hydrochloric acid were measured. The standard heat of formation of the aqueous cerium (III) ion at 25° C is -166.1 ± 0.3 kcal/mole. Heats of solution of cerium (III) chloride in hydrochloric acid are consistent with the existence of a complex CeC1++ having a stability constant of 1 and a heat of complexing of 5.4 kcal/mole.

Jan 1, 1962

By W. W. Weller

Low-temperature heat capacity measurements were conducted, and entropies at 298.15° K were evaluated for sodium monomolybdate (Na2Mo04), magnesium monomolybdate (MgMo04), and calcium monomolybdate (CaMo04). The 298.15° K entropy values were sodium monomolybdate, 38.1±0.3 cal/deg mole, magnesium monomolybdate, 28.4±0.2 cal/deg mole, and calcium monomolybdate, 29.3±0.2 cal/deg mole.

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 P. L. Woolf

Oil was successfully injected into the tuyeres of the Bureau of Mines experimental blast furnace. Determinations were made for the minimum oil addition necessary to permit the maximum available blast temperature of 2,250° F. and the maximum oil rates at blast temperatures of 1,900°, 2,000°, and 2,100° F. From these tests, the upper and lower levels of high-temperature heat input, which limit the smoothly operating furnace, were established. Substantial coke saving was realized with maximum oil injection. Oil-to-coke replacement ratios have been calculated for various conditions, and oil is compared with natural gas and moisture in somewhat general terms. A study of the effect of variations in slag volume and basicity on the sulfur content of the metal at high sulfur loads was made.

Jan 1, 1963

By M. M. Fine

This report describes a Bureau of Mines technical feasibility study of simultaneous reduction and induration of pelletized iron ore to make a product with superior qualities as blast-furnace feed. Highly reduced, physically competent pellets can be made from magnetite and specularite concentrates that contain small additions of bentonite as binder. In batch tests, pellets were dried, surrounded with solid fuel in crucibles, and heated to the reducing temperature. Total iron content of the best products was higher than 80 percent and crushing strength of 1/2-inch metallized pellets ranged up to 600 pounds or more. Comparative tests of several commercial oxide pellets showed a wide range in crushing strengths, but most values were less than 350 pounds. Continuous tests in a rotary kiln resulted in the same degree of reduction, but the pellets had lower crushing strengths because of the limitations in the maximum operating temperature of the small kiln.

Jan 1, 1962