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By M. D. Schlesinger

Experimental data for coal hydrogenation are presented to show that when a vehicle oil produced from coal is present, coal is hydrogenated to the same high conversion whether molybdenum catalyst is impregnated on the coal or intimately mixed with the slurry. Differences in product distribution could be related to the severity of operating conditions. No minimum mixing time was established, but 2 hours was sufficient. Longer periods of mixing, to 14.75 hours, had no effect on the results. The hydrogenation conditions were in the pressure range of 8,500 to 10,000 p,s,i. at 400° to 500° C. Most of the experiments were made in duplicate. The results were obtained with molybdenum concentrations of 0.01, 0.1, and 1 percent. Al the mentioned pressure range and a time at temperature of 15 to 60 minutes, coal conversions higher than 98 percent were obtained.

Jan 1, 1962

By G. E. Johnson

A bench-scale study was made of removing hydrogen sulfide from synthesis gas at elevated pressure by iron oxide impregnated on wood chips. The gas contained 0.02 to 0.06 percent oxygen. The removal of hydrogen sulfide by iron oxide impregnated on wood chips is more efficient at elevated pressure. At constant space velocity, longer periods of operation at 400 p.s.i.g. are possible before the exit gas reaches a given maximum concentration of hydrogen sulfide, compared with 200 p.s.i.g. or atmospheric pressure. In tests at room temperature, 60° C., and 100° C., the most effective removal of hydrogen sulfide was obtained at room temperature and the least effective at 100° C. Dry impregnated wood chips removed only about half as much hydrogen sulfide as chips wetted to a water content of 50 percent.

Jan 1, 1962

By Murray Jacobson

Facts obtained by the Bureau of Mines on the dust-explosion hazard in air of materials used in the plastics industry are presented for 313 samples studied in the laboratory. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum energy required for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent ignition and flame propagation, and, in some instances, on the limiting oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle shape, additives, and resin structure on explosibility are discussed. Relative explosibility of the materials is related to the ignition sensitivity and explosion severity and is denoted by an empirical index. Recognition of the degree of hazard will facilitate adoption of adequate measures for preventing ignition and explosion during manufacturing or processing.

Jan 1, 1962

By Hsun Hu

C. G. Dunn (Geneva1 Electvic Reseavclz Labo,vatory)-Dr. Hu16 has obtained a number of rolling and annealing texture results that partly agree with those of Dunn17 and Dunn and Kohl8 for experiments of a similar nature. I would like to discuss some of the points of agreement as well as some of disagreement and then present some unpublished data as a contribution to the work on textures. Firstly, there is agreement on the components produced during a 70 pct cold-rolling reduction of a (110) [001 ] single crystal; there is agreement on the forma- tion of a (110) [001] recrystallization texture provided recrystallization occurs at 800°C or higher; and there is agreement on the formation of (120) [001] components provided recrystallization occurs below 600°C. There is some disagreement on the low-temperature recrystallization since I also obtained a substantial amount of a (110) [001] component while the author obtained only (120) [001] components. I also discussed the differences between low- and high-temperature recrystallization (which included further annealing changes in the samples on long

Jan 1, 1962

By E. T. Turkdogan, P. Grieveson

The self-diffusion coefficient of oxygen in a liquid silicate slag containing 40 pct SiO2, 40 pct CaO, and 20 pct Al2O3, was determined using the capillary eff;usion technique. Two stable isotopes of oxygen (O17 and O18) were used as tracers. After each diffision run, the slags were reduced with graphite, the evolved carbon monoxide collected and converted into CO,. The oxygen isotope concentrations were obtazned by measuring the (CO2)45/(CO2)44 and the (CO2)46/(CO2) ratios of the gas. It was found that for O17 Exchange of oxygen between neighboring silicate anions, possibly accompanied by the rotation of these complexes, is a probable diffusion mechanism. The exchange of oxygen atoms between holes in the silicate "lattice" may also be postulated. A full understanding of the properties of slags is unlikely unless the structural details are clearly established. Thus properties such as surface tension, viscosity, expansivity, electrical conductivity, ionic mobility, density, compressibility, and so forth, have been studied. Of importance also are the self-diffusion coefficients and the energies of activation for diffusion of the component ions. The self-diffusion coefficients of calcium, 1-3silicon,, sulfur,4 and aluminumS in a ternary silicate slag have been determined with the aid of radio-isotopes. The self-diffusion coefficient of oxygen in such a slag was investigated in the course of the work reported here.

Jan 1, 1962

By Thomas Gleason

Wet scrubbing of fine coal from Thermal dryers poses a number of problems in adapting the gas cleaning equipment for required clean-up of the fine particulate matter. Among then are: 1. The dust In the gases leaving the Thermal dryer cyclone-s is often extremely fine with high percentages of the total dust loading less than one (1) micron in size. 2, The flue gas entering the scrubber is corrosive since the coal fired in the thermal dryer furnace is in the range of 0.7% by weight sulphur or higher. Therefore comparatively high cost stainless steel alloys or corrosion resistant linings are required for a satisfactory service life. 3. Requirements for residual coal loadings leaving the gas e scrubber are continually being lowered while modern coal preparation operation is imposing heavier burdens on the collection system through introduction into the Thermal dryer system of very fine coal previously not recovered. The advent of flotation systems in increasing numbers is typical of this trend 4. The installation of a scrubbing system on Thermal dryers is made primarily to reduce air pollution and product recovery value is of little or no value. Therefore the operating costs, that is, of gas pressure drop and water requirements must be held to a minimum.

Jan 1, 1962

By J. Gordon Parr, L. P. Srivastava

DUWEZ1 has shown that pure titanium and pure zirconium transform martensitically during rapid cooling at temperatures about 30° and 15°C re spectively below their To temperatures. Holden et al.2 determined M, temperatures of Ti-Cu alloys by a metallographic technique applied to isothermally treated samples. Their results, superposed on the McQuillan3 version of the partial Ti-Cu diagram are shown in Fig. 1. Sources of metals were: Titanium: Iodide bar; Foote Mineral Co. Ltd. Zirconium: Iodide bar; Foote Mineral Co. LM. Copper: Spectrographic Standard; Johnson Matthey and Co. Ltd. Alloys were prepared by levitation melting under argon to the following nominal compositions:* 0.5, Quenching, at rates to about 8000°C per sec, was performed by cooling in a stream of helium (99.999 pct pure) a 3/64 in. cube of material previously heated by a tungsten coil in a system operating at. 10-5 mm Hg. Cooling rates below 200°C per sec w were obtained by controlling the current to the heater coil. The specimen was supported on a 32 gage Pt, Pt-Rh thermocouple attached through a DC amplifier to an Edin magnetic oscillograph (Model 8082) with a maximum chart speed of 250 mm per sec. Transformation temperatures were read off the oscillograph charts at the location of the beginning of the thermal arrest. The same specimen was quenched several times, and all runs were repeated on new samples. Regular calibrations of the oscillograph against a potentiometer were made between quenching experiments. The criterion of martensite formation was the effect of surface rumpling. Previously polished samples that showed a rumpled surface after transformation are assumed to have undergone martens itic transformation: transformations of a diffusion type produce no surface disturbance, Figs. 2 and 3. Electrochemical measurements were made in a cell described elsewhere4 whose electrodes were the martensitic and the diffusion-transformed materials in the following electrolytes:

Jan 1, 1962

By W. J. Boone

The Bureau of Mines has programmed for publication a series of Reports of Investigations of studies it has undertaken on low-temperature phase equilibria of several helium-bearing natural gases. This report is the second of a series of papers of the same general title; it is anticipated that additional reports of this series will be published. The advent of a helium conservation program and the prospect of production of helium by private industry, make it especially desirable to publish these data. This report describes phase equilibria related to a natural gas that is processed for helium at the Bureau's Exell Helium Plant (located about 35 miles north of Amarillo, Tex.). Carbon dioxide and water in the gas were removed before making the study; hence the data obtained are representative of the gas stream immediately after similar preliminary treatment in the plant process. Phase equilibrium data were obtained for conditions from -50° to -275° F. and from 100 to 500 p.s.i.a. Analyses of samples were made as follows: For a given run at a selected temperature and pressure, samples of the vapor and liquid phases were analyzed by mass spectrometer, and an additional sample of the liquid phase was analyzed for helium by means of special apparatus (7). 4

Jan 1, 1962

By F. J. Plecity, W. C. Leslie, F. W. Aul

During isothermal recrystallization, the rate of grain growth in dilute Fe-hlo alloys decreased rapidly with increasing Mo content, up to -0.04 at pct, and less rapidly therea-fter. Rate of growth also decreased sharply with time at constant temperature. The observed rates of boundary migration did not cor,espond to predictions of the Lucke-Detert theory. It is proposed that the growth of recrystallized grains is inhibited by clustering of solute atoms at inzperfections in the unrecrystallized matrix. It is now firmly etablished" that the rate of re-crystallization of cold-worked metals, i.e., the rate of growth of recrystallized grains into the deformed matrix, is greatly inhibited by the presence of alloying elements in solid solution. The effect is greatest with the first very small quantity of alloying elements, and additional increments cause much less pronounced retardation of growth. The early papers on this subject were reviewed in Ref. 6. The mechanism of retardation of growth is not clear; only one theory, due to Lucke and Detert? has been advanced. This assumes an elastic interaction between grain boundaries and solute atoms which tends to increase the concentration of the latter in the grain boundaries. Except at very low solute concentrations or at high temperatures, the mobility of the boundary is assumed to be controlled by the rate of diffusion of the accompanying solute atoms. Abrahamson and Blakeney2 have noted a correlation between "recrystallization temperature of binary alloys of iron and the number of d-shell electrons in the solute atoms. There is need for considerably more experimental data on the effect of solute elements on the rate of migration of grain boundaries into the deformed matrix, to provide the basis for an understanding of the annealing process in metallic solid solutions. Only a start has been made in this direction. To avoid unnecessary complications, alloys in which precipitation does not occur should be used, but to produce the maximum effects it is desirable to select alloys with a large difference between the sizes of the atoms of the solvent and solute. For these reasons, alloys of iron and molybdenum sen for this study. MATERIALS AND PROCEDURES A 30-lb. ingot of iron and four similar ingots of Fe-Mo alloys were vacuum melted in magnesia crucibles and poured into cast-iron molds. The molybdenum contents were planned according to the results of Abrahamson and Blakeney2 sothattwoalloyswould fall in the region of rapid change of recrystallization kinetics with change in composition (0.006 to 0.015 and 0.030 to 0.045 at. pct Mo) and two alloys would fall in the region of gradual change (0.18 to 0.24 and

Jan 1, 1962

By Harold W. Lipper

Helium production and shipment reached new peaks in 1.361. The Bureau of Mines produced 727 million cubic feet, 13 percent more than the 1960 record, and shipped 552 million cubic feet, 16 percent more than the 1960 record. Production exceeded demand for the third successive year, enabling the Bureau of Mines to add 174 million cubic feet to the volume stored underground for future use. At the end of 1961, the total volume of helium in underground storage in the Clifside gasfield was 44-7 million cubic feet. Contracts to implement a long-range helium conservation program were completed with four companies, obligating all the contracting authority of $47.5 million a year made available by the Congress. The four companies will finance, build, and operate helium extraction plants to recover from natural gas an annual average of 3.1 billion cubic feet of helium that would ordinarily be wasted when the helium-bearing natural gas is used for fuel.

Jan 1, 1962

By T. P. Meloy

The behavior of slime-sized particles in a flotation cell is neither well documented nor well understood. In general, slimes (or 'fines' as they will be alternatively called in this chapter) have been either ignored, eliminated, or treated empirically. Recently, however, some good experimental and theoretical work has been done that leads qualitatively to a clearer understanding of the problems involved. Fines are small particles that, owing to their smallness, behave differently from larger particles of the same material. The smaller the particle, the larger is its surface-to-mass ratio. The difference in the surface-to-mass ratio for a micron-sized particle and a centimeter-sized particle is 10,000 to 1. For our purposes we shall arbitrarily define any particle less than 10 µ 10-3 cm) as being a fine. This is generally considered the upper limit of colloidal-sized particles. Recently, the field of colloidal chemistry has successfully used the concept of the double layer to explain dispersion and flocculation of fine particles in a static system. Flotation, however, is a dynamic system due both to the turbulence of the liquid and to the coursing of the bubbles through the cell. Further more, a flotation system is a heterogeneous system in which there are a number of different types of particles which interact with one another. A further difficulty is that no two flotation systems are the same for minute quantities of a variety of common chemicals will alter the behavior of the system. These reasons make reproducible experimental results that can ex- plain fine-particle behavior difficult to obtain. In spite of these experimental difficulties, millions of tons of ore containing a large amount of fines are successfully floated every year. For example, at the Morning mill of American Smelting and Refining Co., a galena concentrate that was 42% -6 µ and a sphalerite concentrate that was 33% -9 µ were floated leaving a tailing that was 27% - 9 µ.l Ores that contain fines can generally be divided into two classes. In the first are those in which the valuable mineral tends to slime, such as galena and hematite. In the other class, one or more of the gangue minerals forms the slime; a typical example is barite. Though the problems due to the presence of fines are often the same in handling the two classes of ore, the method of handling them is different because of economic considerations. Nonmetallic mineral flotation is particularly affected by slimes, by either slime-coating effects or excessive reagent consumption. Though a given gangue mineral may not float under the conditions prevailing in the flotation cell, it may still be able to adsorb the collector. I£ it also slimes, a significant

Jan 1, 1962

By D. R. Miller

Internal friction and elastic modulus variations in electrorefined titanium, iodide refined titanium, and alloys of the latter material with oxygen, nitrogen, aluminum, and zirconium were investigated. No oxygen peak was detected with electrorefined titanium but, provided precautions were taken to prevent increases in background damping, an oxygen peak at about 410°C could be resolved with each of the other materials. An additional partially resolved peak was observed at 500°C in a Ti-N alloy. An anomaly in the variation of rigidity modulus with temperature was observed. Possible mechanisms for the formation of any oxygen peak have been discussed. PRATT, Bratina, and Chalmersl investigated the internal friction of commercial purity titanium and alloys of this material containing 1.5, 3.5, and 4.5 at. pct O. With commercial titanium the internal friction curve consisted of two components, a background which increased steadily with temperature and a peak at about 600" C which was due to grain boundary relaxation. In the Ti-O alloys, however, an additional internal friction peak was observed at 430" to 450°C and, since this peak increased in height as the oxygen content was increased, it was thought to be associated with the presence of oxygen. The diffusion of oxygen in titanium at temperatures between 300" and 500° C is believed to have marked effects in its tensile properties2'3 and the present internal friction measurements were undertaken to obtain further information on this diffusion, using material of higher purity than that of Pratt et d. and an apparatus of very much greater sensitivity. In the course of the investigation a number of important limitations on the work of Pratt et al. were revealed and results have been obtained which emphasize the need for ensuring that in this type of experiment, internal friction is independent of strain amplitude and that the values obtained are reproducible. 1) MATERIALS AND APPARATUS The basis material from which the majority of the specimens was prepared was iodide-refined titanium, the major impurities in which were oxygen and nitrogen—the metallic impurities being present at concentrations less than 0.001 at. pct. The hardness of this material after arc melting, forging, and swaging to rods 1/4 in. diameter was Dph = 110. Specimens 10 in. long and 0.020 in. (0.51 mm) diameter were prepared from these rods by further swaging and wire drawing and were finally annealed in vacuo (5 x 10-6 mmHg) for 24 hr at 800°C. The oxygen alloys were prepared from iodide-

Jan 1, 1962

By T. J. Koppenaal, M. E. Fine

The critical resolved shear stress of aCu-A1 single crystals has been investigated as a function of composition, testing temperature, and strain rate. The strength, and its temperature and strain rate dependency increase markedly with aluminum content. The solid solution strengthening at 4.2°K is much larger than at room temperature. The activation energy for the low temperature dislocation cutting process increases from about 0.17 ev for a 0.5 at. pct A1 alloy to about 0.50 ev for a 14 at. pct A1 alloy. This result is attributed to an increase in the width of extended dislocations due to the known decrease in the stacking fault energy. In addition, the activation volumes at 4.2 and 77°K decrease with aluminum additions. Concerning the solid solution strengthening in the 296° to 373°K range, no definite conclusions are reached, but it is suggested that subgrains and cutting of subgrains are important. In a previous paper,' the authors reported that adding aluminum to copper produces two types of strengthening: a yield point effect and an increase in the lower yield stress. This behavior is illustrated in Fig. 1 by shear stress-shear strain curves of furnace-cooled single crystals of pure copper and Cu-14 at. pct A1. The yield point effect, At, was thoroughly studied previously1 and shown to be associated with short-range order. The present paper reports an investigation of the lower-yield stress in aCu-A1 single crystals as a function of composition, testing temperature, and strain rate. EXPERIMENTAL PROCEDURE Single cryski1 tensile specimens were prepared in the same manner as previously described.l Briefly,

Jan 1, 1962

By C. Z. Serpan, L. J. Wittenberg

The density of liquid plutonium was determined, by a pycnometm'c technique, from 664 to 788°C and exhibited a temperature dependence, which could be expressed as:. P= C17.63 - 1.52 x 10-"t] +0.04 g per cc where t = OC. These density values compare favorably with the values previously obtained by a technique utilizing Archimedes' principle. The apparatus and method were evaluated when the densities 0.f molten tin and bismuth were measured and found to be in agreement with accepted literature values. PLUTONIUM or an alloy of plutonium in the liquid state has been proposed as a fuel for a fast-breeder type nuclear power plant.' Since knowledge of the liquid density of plutonium is required for the proper design of such a system, this study was undertaken. In addition, the density and volume expansion coefficient of liquid plutonium are of interest for comparison with these same properties of the six allotropic modifications of the solid metal. Comstock and GibneyZ were first to report a value for the density of liquid plutonium. The value for only one temperature, 665"C, was calculated from data obtained by the radiography of the meniscus, Fig. 3. Recently, the density at a series of temperatures has been reported by Knight,3 who obtained his values by using a differential volumeter, and by 01-sen, Sandenaw, and Herrik, who obtained their values from measurements of the loss in weight of a tungsten bob immersed in the liquid. The density of liquid plutonium reported here was determined by a vacuum pycnometer method. In an evacuated system, the tips of calibrated tantalum pycnometers were lowered beneath the liquid sur-

Jan 1, 1962

The various functions of public relations are playing an increasingly important part in the activities of the many companies now engaged in oil exploration in Australia.Several of the larger exploration companies, notably West Australian Petroleum Pty.Limited, Ampol Exploration Limited, Caltex Oil (Australia) PtSr: Limited and Australian Oil and Gas Ltd. (and its American Associate Union-Kern), employ staff or consultant public relations specialists. In, most of the other companies now exploring in Australia, public relations are handled within the company, directed from the highest executive level.The object of public relations in.the oil industry is. to create in the public mind an impression favourable to the industry as a whole and'the company -or group of companies with which the public relations officer is associated.

Jan 1, 1962

By J. P. Capp

The Bureau of Mines conducted field-scale experiments in underground gasification of coal with oxygen-enriched air. A path about 140 feet long was linked at the rate of LO feet per day through a coalbed hydraulically fractured with a mixture of starch gel and sand. During the best gasification period, which extended for 2-1/2 days, 785,000 std. c.f. per day of 124-B.t.u. gas was produced. In other periods the heating value at times was almost 300 B.t.u. per std, c.f,, but sustained production of such gas was not achieved. During gasification, a total of 50 tons of coal was gasified and 114 tons of coal was carbonized. Approximately 12 million B, t .u. per foot of nominal path was recovered at the surface.

Jan 1, 1962

By B. A. Rose

Coal is being thermally dried in ever increasing tonnages today. Because of fire and explosion hazards, it is important that drying equipment be designed for maximum safety in operation. It is well then that we review dryer design and operation to bring out those features and operating practices which will provide maximum safety to equipment and personnel. This paper presents the author's views regarding the fundamental requirements for safety and explains the Heyl and Patterson approach to the meeting of those requirements in the design and operation of their dryer.

Jan 1, 1962

By John A. Brooks

The description of a phosphate flotation operation is repeat information for many people, except for variations in flow sheets. This paper is written to show the variations in flows, and to give enough. of the overall flows to allow anyone not familiar with the operation to be able to formulate a fair idea of the operations.

Jan 1, 1962

By Robert Hall

The Lynch Creek beryllium-tungsten prospect was investigated as part of the domestic beryllium resource studies by the Bureau of Mines. This prospect is in the Birch Creek mining district, Lander County, Nev., 9 airline miles south of Austin. A tungsten mine was operated intermittently from 1952 to 1957. Beryl was identified in the pegmatite dikes in 1960, and the lode claims were relocated. No beryl has been produced. Rocks in the area are Paleozoic sediments2 cut by pegmatite and aplite dikes and quartz stringers. Beryl occurs in random pockets, as disseminations throughout the dikes, and in occasional pockets in the quartz stringers.

Jan 1, 1962

The Geograph is a revolutionary seismic system involving special techniques in combining the use of FIT magnetic tape with shock wave echoes created by a weight dropping system.The idea of- weight dropping as a- source of seismic energy is not a new,.,oxie. Records 'indicate òa pos'sihle use of falling weights as early as .1929. 'Dr. Burton McCollum began his experiments in 1938, but it wasn't until 1951 that the method was first proven useful.The first weight dropping crew began commercial operations in Edwards and Sutton .Counties of West Texas in 1953. By 1962, more than '40 weight drop-ping.crews have come into existence with operations in the United States, Canada, Algeria, Iraq, Argent na,òSpanish West Africa, Tunisia, Qatar, Niger Morocco and Libya by most major oil companies and larger independent oil companies. .

Jan 1, 1962