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Jan 1, 1969

By George D. Haley

This report will be given in two sections. The first sec¬tion outlines techniques and equipment to form almond shaped fluorspar briquettes by means of briquet presses, and the second section outlines techniques of the balling disc. PART I - BRIQUET PRESSES Fluorspar has been briquetted for a number of years and the so called "peach pit" briquet is known to many steelmen. Present production is estimated at over 100,000 tons annually. Slide 1 shows an assortment of various sizes and shapes of briquettes. It is possible to form fluorspar into almost any configuration of briquet. For safety on the melting floor, pillow type briquets are preferred. Ease of mechanical handling and durability of the product are facil¬itated by an almond shape. The dimensions of the almond can vary from 1-in. to 1-1/2-in. in length, from 13/16-in. to 1-in. in width and from 1/2-in. to 1-in. in thickness. The type of equipment to pro¬duce almond shaped fluorspar briquettes is shown in Slide 2. Here we have a Komarek-Greaves and Company 300 ton briquettor equipped with almond rolls. This machine is capable of producing fluorspar briquettes at a rats of 30 tons per hour with power consumption of 35 hp per ton par hour.

Jan 1, 1969

By Manuel Gomez

The Bureau of Mines used data from 31 core samples to develop prediction equations for evaluating chemical and carbonization properties of six seam units in a lignite deposit approximately 2 miles wide and 8 miles long in the Wilcox Formation of central Texas. Statistical response surfaces, based on core analyses, were computed for 14 parameters indicative of lignite quality. These computed surfaces, and their mathematical equations, can be used to predict values of the selected properties of the lignite seams at any desired surface coordinate position between core hole locations. The wide range of application shown by this study indicates that the methods of statistical regression analysis may be useful to evaluate large deposits of lignite or higher rank coal.

Jan 1, 1969

By N. Plint, E. T. Pinkney

Copper segregation developments within the Anglo American Group are described with particular reference to the work of the TORCO Project Team. Some radical differences have been adopted in the mechan-ical approach as compared with methods used by previous workers. Most important among these are the following: (1) The heating unit is a fluidized-bed roaster. (2) A moving bed segregation chamber is used in which a packed bed of heated ore, to which reagents have been added, moves slowly downwards under gravity and is discharged at a controlled rate by means of a suitable valve mechanism. (3) The quantities of reagents used (sodium chloride and some form of carbon) are only a small fraction of those recommended by other investigators. (4) Retention times of only 2 min have been satisfactory for the complete segregation of many types of ore. Project TORCO is the code name given by Anglo American Corp. of South Africa, Ltd., to the investigation undertaken in Zambia to develop a plant capable of treating large tonnages of refractory copper-bearing ores by the segregation process. The process has now been under investigation for six years (1960-66) and during that period work has progressed from bench-scale laboratory tests through small-scale pilot-plant work to a 500-tpd commercial pilot unit. Test work has been carried out mainly on the ores of the Zambian Copperbelt and results have been encouraging. Recoveries on the order of 90% have been obtained on all Copperbelt ores tested with high concentrate grades. PRELIMINARY INVESTIGATION Laboratory scale segregation test work on Nchanga banded sandstone ore and oxidized ore from Kansan-shi was originally conducted by Professor Maurice Rey. SociCtC Miniere et Mktallurgique de Pefiarroya, in 1957. Both ores responded favorably to the process. In November, 1960, the consulting engineers of Anglo American Corp. of South Africa, Ltd., initiated preliminary investigations on the application of the segregation process to Copperbelt ores. In early laboratory work, samples were heated in a closed, externally heated tube furnace for one hour at temperatures ranging from 800 to 830°C. The free moisture content of the ore feed was 4% and reagent additions were 0.5% salt and 1.0% coal. Both salt and coal were pre-crushed to -48 mesh Tyler.* All samples except an ore from the Bancroft mine responded well to the process and recoveries of over 90% were obtained. The presence of dolomite was responsible for the relatively poor recoveries from the Bancroft ore, as tests on one of the other ores with additions of calcite or dolomite confirmed. Recoveries dropped from 94 to 45% Grades of all the rougher flotation concentrates produced were low at 10-15% copper. The laboratory investigation was then followed up on a pilot-plant scale. An attempt was made to carry out the segregation process in a coal-fired 5-ft-diam fluidized-bed roaster. The feed consisted of a banded sandstone from Nchanga to which 0.5% sodium chloride had been added. Reducing conditions were maintained in the roaster by the addition of coal in excess of that required for heating the feed. The excess coal and added salt constituted the segregation reagents and the temperature of the bed was held at approximately 750°C. Recoveries of copper and grades of concentrates were low. The reasons for lack of success were: (1) The reaction is a gaseous one and a fluidized-bed roaster is therefore unsuitable as a segregation unit. (2) Coal in excess of that required for heating was introduced into the fluidized bed and under these conditions some of the copper would be reduced in situ. The term "reduced in situ" is used here to describe any copper mineral reduced to the metallic state in its original site within the ore particles. If this copper is to be recovered by subsequent froth flotation it must first be liberated from the gangue by grinding or some other method which, in practice, is usually not feasible on ores of this type.

Jan 1, 1969

By H. W. Schadler

The superplastic behavior of low carbon and manganese bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests are reported which indicate that high strain rate sensitivity (>0.5) and adequate elongations are achievable in ultrafine-grained steels 1 to 2 p, but at strain rates which are not commercially attractive. It has been demonstrated that the fine grain size is retained after long times and high strains if the temperature is kept within the range of the two-phase (a + ?) field. INTEREST in superplasticity has been stimulated by the desire to: 1) understand the origin of, and mechanisms responsible for, the large uniform elongations observed, and 2) exploit this property for commercial advantage in metal forming operations. Although the Zn-22 wt pct Al alloy presently being studied as a model material1-5 may find application in sheet forming and extrusion, the potential of super-plasticity should best be realized in large tonnage materials, such as steel and aluminum alloys. The degree of superplasticity in low-carbon and manganese-bearing steels has been evaluated. The results of elevated-temperature stress-strain rate and elongation tests on ultrafine grain size material are reported. Avery and Backofen6 and Hart7 have shown that geometrically stable flow leading to extensive uniform elongation in the tension test is associated with high values of the strain rate sensitivity, m, defined: Lozinsky had reported that titanium and zirconium experience permanent deformation if subjected to a constant load and cyclic heating through the temperature range of the phase transformation. Although strain rate sensitivities in excess of about 0.2 had not been reported previously for steel, permanent deformation had been observed11-13 in a wide variety of steels subjected to a constant load and cyclic heating through the temperature range of the a-? phase transformation. Thus by analogy, steel could be expected to exhibit high strain rate sensitivity but only in the a + ? condition. High strain rate sensitivity has been observed at 650°C (a + Fe3C), but not reported as such, by Bailey, Dickenson, and pearson14 in 1931 at a strain rate of about 10-9 per min. It then remained to determine whether high tensile elongations would be observed in a rate-controlled test at constant temperature and at what strain rate strain rate sensitivity values greater than 0.5 would be observed. Since previous experience8 had indicated the importance of fine grain size to realizing high m at reasonable strain rates, it was first necessary to produce an ultrafine grain size and then keep the grains from growing during the test. The results of this investigation show that fine grain size can be readily produced16 and maintained by restricting the temperature of testing to below the ? transus. Further, superplasticity (high m and large uniform elongation) is observed. However, the strain rate range is only marginally useful for commercial forming operations with the finest grain size produced. MATERIAL The material investigated initially was a 1.9 wt pct Mn, 0.42 wt pct C, hot-rolled bar previously used by Low and Turka1015 and available in the laboratory. The 0.500-in. round was cold-rolled to a 0.090-in. flat, annealed for 4 hr at 850°C in argon, air-cooled, and cold-finished to 0.050 in. Subsequently, four additional steels of the compositions given in Table I were investigated to explore the effects of manganese, carbon, and test temperature on the observed stress-strain rate behavior. These steels were melted under argon, cast to 0.75 by 2 by 5 in. slabs, hot-rolled at 850°C, surface-finished to 0.13 in., and cold-finished to 0.050 in. Sheet tensile specimens 0.200 in. x thickness with 1- or 2-in. gage length were cut parallel to the rolling direction. Table I also includes the nominal transformation temperatures for the AISI 1340 and the four experimental steels. EXPERIMENTAL PROCEDURE Production of Fine Grain Size. Ultrafine grain size (1 to 5 p) was considered essential for this studv. Grange16 has described two techniques for producing

Jan 1, 1969

By A. R. Calawa, T. C. Harman, M. Finn, P. Youtz

A study has been made of the growing, annealing, and diffusion parameters in PbSe, Pb1-ySnySe, and Pb1-xSnxTe. Single crystals of these materials have been grown using the Bridgman technique. For all of the above materials the as-grown crystals are p type with high carrier densities. To reduce the carrier concentration and increase the carrier mobility, the samples are annealed either isothermally or by a two-zone method. From isothermal anneals, the liquidus-solidus boundary on the metal-rich side of the stoichiometric composition has been obtained for some alloys of Pb1-xSnxTe and on both the metal- and seleniunz-rich sides for PbSe and alloys of Pbl-ySnySe. In Pbo.935 Sno.065 Se carrier concentrations as low as 5 x1016 Cm-3 and mobilities as high as 44,000 sq cm v-1 sec-1 at 77°K have been obtained. Inter diffusion parameters mere also studied. The ddiffusion experiments mere identical to the isothermal or two-zone annealing experiments except that the samples were removed prior to complete equilibration. The resulting p-n junction depths were determined by sectioning and thermal probing. Inter diffusion coefficients for various temperatures were calculated for both PbSe and Pb0.93Sn0.0,Se. RECENTLY, there has been considerable interest in the PbTe-SnTe and PbSe-SnSe alloys with the rock salt crystal structure. The unusual feature of these systems is the variation of energy gap EG with composition. Several investigations1-3 have shown that EG for the lead chalcogenides decreases as the tin content increases, goes through zero, and then increases again with further increase in tin content. The possibility of obtaining an arbitrary energy gap by selecting the composition is an especially attractive feature of these alloys for applications involving long-wavelength infrared detectors and lasers. In addition, some unusual magneto-optical, galvanomagnetic, and thermomag-netic effects should occur for alloys with low band gaps. If uncompensated low carrier density crystals can be obtained, then a small carrier effective mass, a large dielectric constant, and the resultant high carrier mobility should yield enormous effects at low temperature in a magnetic field. The relative variation of the energy gap with pressure should also be very large for these low gap materials. The primary purpose of this paper is to provide some information concerning the preparation of low carrier concentra- tion, high carrier mobility, and homogeneous single crystals with a predetermined alloy composition. I) DETERMINATION OF ALLOY COMPOSITIONS In all of the work described in this paper, the composition of lead and tin chalcogenides in the alloys was determined by electron microprobe analysis. Separate X-ray spectrometers are used to make simultaneous intensity measurements of the Pb La1 and Sn La1 lines emitted by the sample under excitation by a beam of 25 kev electrons focused to a spot about 2 µm in diam. These intensities are compared to the intensities of the same lines emitted by standards under the same conditions. The standards used are the terminal compounds of each pseudobinary system, i.e., PbTe and SnTe for Pbl-xSnxTe alloys, PbSe and SnSe for Pbl-ySnySe alloys. The composition of the sample is then obtained from theoretical calibration curves which relate the weight fractions of lead and tin in the alloy to the measured ratios of X-ray intensities for the sample and the standards. The lead and tin calibration curves for each alloy system were calculated by using corrections for backscattered electrons,4 ionization,5 and absorption,6 and assuming that the atom fraction of tellurium or selenium in the sample and standards is exactly +. Results obtained by using the microprobe are in good agreement with those obtained by wet chemical analysis. II) CRYSTAL GROWTH FROM THE VAPOR Early work on the vapor growth of PbSe was carried out by Prior.7 He used small chips of Bridgman-grown single crystals as the source material and frequently converted the whole charge of a few grams into one crystal. In the present work, vapor growth occurred using a metal-rich or chalcogenide-rich two-phased alloy powder as the source material. Small, nearly stoichiometric crystals are formed on the walls of the quartz tube. The procedure will now be described in detail. Initially, a 100-g charge containing (metal)o.51(chalco-genide)o 49 proportions or (metal)o.49(chalcogenide)o. 51 proportions of the as-received elements in chunk form are placed in a fused silica ampoule. After the ampoule is loaded, it is evacuated with a diffusion pump and sealed. The sealed ampoule is placed in the center of a vertical resistance furnace. The region containing the ampoule is heated to about 50°C above the liquidus temper-ature for the particular composition used. After about one-half hour at temperature, the elements are reacted and the molten material homogenized. The ampoule is quenched in water. The quenched ingot is crushed to a coarse powder for vapor growth experiments and to a fine powder for the isothermal annealing experiments which are discussed in a later section. Vapor growth experiments were carried out using the powdered, metal-rich or chalcogenide-rich alloys

Jan 1, 1969

By K. Koneko, T. Nokoyama, S. Shibato

SEYBOLT et al.' have detected various silica films formed on a 3 pct Si-Fe alloy after heating at low oxygen potentials with the electron diffraction method, and they have made some observations on the H,0/H2 ratios required to form them. The purpose of this note is to describe the structure of the oxide film formed on either mechanically or electrolytically polished surfaces of a 3 pct Si-Fe alloy containing small amounts of manganese after heating at low oxygen potential. The samples were prepared from a Si-Fe alloy made in the laboratory using electrolytic iron, 76 pct ferrosilicon, and 76 pct ferromanganese, vacuum-in-

Jan 1, 1969

By C. D. Hall, F. E. Dollarhide

Fluid Ioss agent.s for crude oil and for water have been studied in dynamic tests. A treatment using a spearhead with a fluid loss agent followed by plain fluid appears feas ible in crude oil, but not in water. An equation for spearhead depletion shows that spurt loss relative to fracture width must be low, if the portion of spearhead fluid in the treatment is to be small. The presence of colloidal matter in crude oils aids the fluid Ioss agent. Unlike in kerosene, where flow limited the agent deposition, in crude oils the filter cake continually formed and leak-off declined. The volume-time relation varied somewhat for different crudes, but was best described by a square root of time function. Spurt loss was inversely proportional to agent concentration. After the fluid loss agent initiated the filter cake, the crude oil colloids built on it effectively. A 2-minute or a 5-minute spearhead with double the normal agent concentration gave the same fluid Ioss curve as the same concentration did for a 30-minute test. The agents tested in water gave fluid Ioss plots on which, for the first few minutes, volume was proportional to the square root of time, but later became proportional to time. For fracture area calculation the customary square root of time function is a satisfactory approximation. Leak-off rates and spurt losses were higher in water systems than in oils. The spurt Ioss tended to be inversely proportional to concentration. In spearhead tests, the filter cakes were not eroded by water flow. However, the rather high spurt loss values make spearhead treatments impractical for water-based fluids. Introduction The effects of dynamic testing conditions on the performance of fluid loss agents in kerosene have been studied previously.' We have extended the work to include crude-oil- and water-based fracturing fluids. An understanding has been gained of the mechanisms of formation and functioning of the filter cakes of fluid loss agents. The practical aspects of evaluating performance of agents in relation to fracture area calculations also are considered. The feasibility of using the fluid loss agent in a spearhead stage of the treatment is examined further for both types of fluids. Experimental Procedure The dynamic fluid loss tests were performed in an apparatus similar to the high-pressure apparatus described in a previous publication.' A fracturing fluid was circulated over a rock surface located in a closed pressurized loop. The fluid flowed axially over the cylindrical surface of a core 2 in. in diameter X 3.5 in. long, mounted (with the flat ends sealed off) in a pipe, with 0.117 in. annular clearance. The filtrate was collected in a central hole in the core and led through valves to graduated cylinders. Provision was made for changing quickly the circulating fluid during the test (spearhead runs) without interrupting the filtration pressure. The only modifications were to add heating tapes and water jackets for the tests with crude oils, all conducted at ISOF, and to change all parts exposed to the test fluid to stainless steel for the tests with water-based fluids. The latter tests were made at room temperature, 80F. Three crude oils were tested. A mixed crude, obtained from a local refinery, contained a considerable amount of light ends. For safety reasons, it was stripped to 250F vapor temperature before use in the fluid loss tests. The other two oils were used as obtained from lease tanks. One was a greenish-brown, 37" API paraffinic crude, and the other was a black, 32" API asphaltic crude. The fluid loss agent for oil, here designated for brevity as Agent A, was Adomite@ Mark II*, a granular solid commercial agent, the same as previously tested in kerosene.' Three different compositions of fluid loss agents were tested in Tulsa tap water. Agent B was adomit& Aqua*, a solid commercial fluid loss agent, comprising clays and hydrophilic gums principally derived from starch. Agent C was a mixture of three parts of Agent B with two parts of silica flour. Agent D was Dowel1 J137, a mixture of guar gum and silica flour. The test cores were cut from contiguous blocks of Berea or Bandera sandstones. For the oil tests, the cores were oven dried, evacuated, saturated with kerosene, and the kerosene permeability was measured. The cores used with the water-based fluids were pretreated by saturating with 3 percent calcium &loride solution to minimize pemeability damage by the fresh water due to clay migration. The

Jan 1, 1969

By K. I. Savage, S. C. Sun

This paper describes a process developed to recover coal, clays and pyrite from coal wastes. The process consists of fine grinding followed by coal and pyrite flotation which leaves the clays in the flotation pulp. A bituminous coal refuse containing 10% sulfur and 30% carbonaceous material was treated by this method to yield a coal product containing 4% sulfur, 10% ash; a pyrite product containing 45% sulfur (84% FeS2), 1% carbonaceous material; and a clay product containing 2% sulfur (3.5% FeS2). The coal yield was about 89%. The pyrite yield was about 77%. The process steps may be entirely flotation, or gravity separation (hydrocycloning) may be used to increase the pyrite : coal ratio in the flotation feed. Cost estimates for the process show a profit of $2.28 per ton of low pyrite grade refuse, but these do not include labor, maintenance, overhead and plant depreciation. The development of this process consisted of three parts: (1) exploratory tests, (2) op-timazation tests and (3) confirmatory tests. The objectionable qualities that sulfur imparts to coal have been commented upon from early times, and they have become more objectionable as the uses of coal have grown. In whatever form coal takes — raw, carbonized or gasified —the sulfur content remains objectionable, and therefore its compounds are removed as completely as possible. It has long been known that sulfur occurs in coal in different forms. In 1861, sulfur was said to exist in the state of sulfuric acid in combination with a base; in combination with iron as iron pyrites; as bisulfides of iron; and in combination with the organic elements of coal.' Pyritic sulfur is a term loosely used to cover the sulfur associated with iron in its various forms. The mineralogically recognized forms are pyrite (FeS2), pyrrhotite (Fe 1-x S) and marcasite (FeS2). The particle sizes of pyrites vary widely. Isolated grains of marcasite smaller than 15 microns have been found disseminated through coal.2 Hair-like "veins" of pyrite filling cracks in vitrain have been found. At the other extreme, lumps or nodules of pyrites large enough for removal by hand picking have been encountered. Organic sulfur, unlike pyritic sulfur, does not exist as discrete particles, but is instead intimately associated with the coal structure and thus it is impossible to remove it or reduce its concentration by physical or mechanical means.2 In the preparation of coal for its various markets, the pyrite minerals (pyrites) are separated from the raw coal feed. This separation process concentrates the pyrites in the tailings or other waste products. It would be desirable to recover these pyrites for three reasons: (1) Pyrites are potential sources of sulfur and iron. In 1967, for the fifth consecutive year, Free World consumption of sulfur exceeded production.3 Propelled by the shortage, the domestic price of sulfur has risen from $24 to $38 per long ton (bright). (2) The refuse, when placed in piles, becomes ignited. The pyrites (FeS2) bum, giving off SO,. Thus, the pyrites are a cause of air pollution. (3) Also, the pyrites undergo chemical reaction when exposed to air. The refuse is leached by waters which result in stream pollution due to the water-soluble iron and acidic reaction products. Coal refuse also contains coal minerals and clay minerals. Therefore, any process for recovering the pyrites must successfully separate them from the coal and clay minerals. In the study discussed here, ten different bituminous coal refuse samples were successfully upgraded in pyrite content. These samples represented a wide variety of coal waste materials from Pennsylvania and other states. The variabilities of the sulfur and coal contents are shown in Table I. The extremes are Sample J, a high sulfur-low coal, and Sample B, a low sulfur-high coal. Definitions of some of the symbols or terms used in this report are given below: Mesh size—Tyler standard mesh screen sieves with an opening based on the square root of two. Fe —Indicates iron, as determined by a stannous reduction-dichromatic oxidation method. S—Indicates sulfur, as determined by the ASTM "Eschka" method for sulfur in coal.

Jan 1, 1969

By F. G. Robb, D. N. Madge

This paper details some of the specifications and problems associated with implementing on-line control of a potash concentrator. The computer system described has the capability of three levels of control, including DDC with a single central processor. The system is also capable of on-line program compilation and modification through an extension of vendor utilities. The system is now in operation.

Jan 1, 1969

By J. L. Konchesky

The Bureau of Mines investigated the main reactions of coal gasification by steam. Coal (minus 70 mesh)-water slurry was fed into a laboratory-scale tube-coil gasifier to show the effects of residence time (0.6 to 1.1 sec), steam-coal ratio (2 to 11 lb/lb), and temperature (1,600° to 1,900° F), at about 1-1/2 atm. Devolatilization was very rapid: about 70 pet of the coal's volatile matter evolved within 0.6 sec at about 1,600° F; temperature increase released more volatile matter until about 95 pct was driven off at 1,900° F. Devolatilization was not increased by raising steam concentrations and was only slightly increased by extending residence time. Below 1,600° F, there was no evidence of the steam-carbon reaction, but at 1,900° F more than 80 pct of the coal's fixed carbon was converted to gas; the conversion was increased Significantly by increased residence time and steam concentration. The water-gas shift reaction occurred simultaneously with devolatilization, and the steam-carbon reaction, approaching equilibrium with increased residence time and temperature and decreased steam concentration.

Jan 1, 1969

By R. K. Datta, T. S. Davis

YVO4:EU, excited under 3650A radiation, shows a marked increase in total brightness with in~rease in temperature. At 25°C the response to 3650A radiation is about 48 pct of its maximum response which occurs at about 350°C, Fig. 1. In an attempt to explain the phenomenon, one of the present authors' (R.K.D.) investigated the diffuse reflectance spectra of the phosphor at different temperatures (up to -150°C) and was unable to observe any significant change to which the increased brightness could be reasonably ascribed. Since then diffuse reflectance spectra at elevated temperatures have been obtained in this laboratory using an improved device. A significant decrease in the diffuse reflectance of a phosphor in the ultraviolet region—especially in the longer wavelength region—at -300°C has been observed. The purpose of this note is to describe the device used for high-temperature reflectance measurements and to explain the increased brightness of YVO4:Eu phosphor at elevated temperatures under 3650A excitation. Experimental. YVO4 and YVO4:Eu samples were prepared as previously described.' The elevated-temperature reflectance spectra were obtained with a Cary 14 spectrophotometer equipped with a diffuse reflectance accessory and a ring collector. CaF2 was used as the standard. The cell used

Jan 1, 1969

By R. D. Nelson, S. D. Dahlgren

The conditions of temperature, strain rate, and total strain favoring deformation by grain boundary sliding, slip, or deformation with concurrent recrystallization were evaluated for alpha plutonium. Grain boundary sliding and slip were studied by examining structures formed on polished surfaces with 4.5 pct compressive deformation. The conditions required for recrystallization were determined from compressive deformation us time curves. At 110" C and at a strain rate of 10&apos;per min, deformation was almost exclusively by grain boundary sliding whereas slip was the predominant deformation mode at -10°C and lo-&apos; per min. Defarmation at intermediate tenzperatures and strain rates produced structures showing mixtures of grain boundary sliding and slip. Recrystallization occurred concurrently with deformation only after a critical strain was reached. About 14, 6, and 3 pct strain was required at 105", llO°, and lZO°C, respectively, before recrystallization started, irrespective of the strain rate in the range of lo-&apos;1 to 10&apos;4 per nzin. L HE temperature and strain-rate dependency of the modes of plastic deformation were evaluated for high-purity as-cast alpha plutonium. The techniques used to study slip and grain boundary sliding were similar to those employed previously for alpha plutonium by Bronisz and Gorum,&apos; and spriet.&apos; Recrystallization was investigated using the methods reported by Nelson.3 Bronisz and Gorum&apos; found that slip occurred on more than one slip system at room temperature, and suggested that grain boundary sliding also contributed to the deformation. spriet2 found that deformation was predominantly by slip at room temperature, and observed one to three orientations of slip traces in individual grains. In addition, he deformed polished samples at 10O° C, but concluded that the deformation character of alpha plutonium at 100° C and at room temperature were not essentially different. Several investigators reported that twinning was only occasionally observed.1&apos;2&apos;4 Nelson3 recently found in creep tests that high-purity alpha plutonium would recrystallize concurrently with compressive deformation at temperatures between 25" and 115°C. EXPERIMENTAL PROCEDURE Electrorefined plutonium having less than 300 ppm total impurities was received from Los Alamos Scientific Laboratory in the form of +-in. diarn cast rods. Major impurities were americium, <I00 ppm, and tungsten, (60 ppm. Less than 25 ppm each of other impurities were present. The rods were cut into right half-cylinders 0.35 in. long and 0.25 in. in diam, and the flat faces along the cylinder axes were metal-lographically polished. To avoid loss of the metallo-graphic polish by oxidation, the polished samples were deformed in a silicone fluid heat treating medium contained in a chamber evacuated to a pressure of lo-&apos; torr. Deadweight loading was used to compress the samples between 4.5 and 20 pct at strain rates between 10"4 and lo- &apos; min-&apos;. Strain rates were determined by dividing the total deformation by the elapsed time of the test, even though the strain rate was not constant during deformation. Curves of strain vs time for samples deformed with a constant compressive stress3 show that the strain rate changes by less than a factor of four during the testing of a given sample, which is small compared to the three orders of magnitude change in strain rate investigated. Two samples were loaded into an ordinary metallographic mounting mold and impacted by striking the mold piston with one blow of a 2-lb hammer. Deformation temperatures for the two impact samples were 25" and 90°C. The samples, following deformation, were washed in carbon tetrachloride and their polished and deformed surfaces were immediately inspected metallographi-cally. Subsequently, the deformation structures were replicated with acetate replicating tape for later electron microscope examination, and the samples were then repolished and etched to reveal the microstruc-tures of the deformed metal. Second-stage carbon replicas were prepared from decontaminated acetate replicas using the procedure developed by Miller, Bierlein, and astel.&apos; Additional samples, which were 0.35 in. long by 0.25 in. in diam, were used to obtain constant load deformation vs time curves. These samples were deformed 10 to 20 pct with loads of 15 and 20,000 psi at 120°C; 30, 45, and 55,000 psi at 110°C; and 20 and 30,000 psi at 105°C. Samples were polished and etched to determine whether or not recrystallization or twinning had occurred during deformation. RESULTS AND DISCUSSION The experiments showed that alpha plutonium deforms by grain boundary sliding, slip, and deformation with concurrent recrystallization. Deformation by twinning was insignificant. Metallographic examination of polished and deformed surfaces revealed grain boundary sliding and slip. The start of recrystallization was ascertained from constant load deformation vs time curves. Deformed surface structures of samples compressed 4.5 pct under four different conditions of temperature and strain rate, Fig. 1, show how the deformation mode changes from predominantly grain boundary sliding to predominantly slip with increasing strain rate and decreasing temperature. Deformation at 110°C and 10" 4 min-&apos;, Fig. l(a), was predominantly by grain boundary sliding. Only a few slip traces can be seen in Fig. l(a).

Jan 1, 1969

Jan 1, 1969

By John Ward Smith

The Bureau of Mines derived equations expressing the theoretical relationship between density of oil-shale rock and its organic content. Effects on theoretical shale density produced by variations in mineral composition and organic matter properties were evaluated. The theoretical relationship was extended to relate oil-shale density to oil yield in both oil weight and volume units by considering the fraction of organic matter converted to oil and the specific gravity of the oil produced. Corollary equations relating organic content by volume to organic content by weight and to oil yield were developed. The general relationships apply to an oil-shale deposit uniform in character. Application of the theoretical relationships to Green River Formation oil shales was demonstrated.

Jan 1, 1969

By Johnson M. W

Factual data about the sedimentation in the Newcastle Coal. Measures are presented. Data concerning the total coal measure sequence (isopachs, sand /shale ratio and total coal thickness variation), data about three coal seams (Borehole, Dudley and Victoria Tunnel) and data about interseam con- glomerate units are discussed. From this data conclusions are drawn about the coal measure environment. The western edge of the coal basin, the Lochinvar Dome, although a high feature was apparently stable during coal measure time. Despite its height it apparently supplied little sediment to the basin. The northern and north-eastern edge, which was unstable, suppl- ied most of the coarse detritus including the conglomerates to the basin. The conglomerates show patterns of fluvial origin but after a period of "normal" variations in pattern they become restricted to two parallel zones evidently tectonically controlled. Deposition of conglomerates is episodic and separated by periods of coal formation when deformation was apparently slight. Formation of each of the three seams considered followed a rather similar pattern - each shows development of thick coal around the basin edge and poor thin coal in the "axial" region of the present synclinal structure. Evidence of in-situ formation of some areas of the seams is discussed and periodic deformation of the basin during coal measure time is postulated.

Jan 1, 1969

By Robert M. Lewis

Chemically, mica is a complex silicate of sodium, potassium and aluminum. There are no important uses of mica where the chemical analysis is important, except that in some uses of ground mica, the content of iron oxide present as an impurity must be kept to a very low limit. Muscovite mica is frequently found containing black and red "stain" as a homogeneous part of the books or sheets. In most cases this stain or impurity is magnetite or hematite. Some mica contains impurities deposited by infiltration. This is commonly a red stain, less often brown or white. The best mica is free from all such impurities, and the greater their content, the less value does the mica have.(1) It is because of these undesirable impurities that a large segment of the fine ground mica industry relies on weathered pegmatites and alaskite ores as a source of raw material. The mica concentrates obtained from these ores are relatively clean and require moderate beneficiation to meet color and density specifications. One need only to observe the stained and decrepitated condition of the mica recovered from mica schist to appreciate the challenge that processing this material presents. Despite these adversities there are several advantages to be gained by mining and processing mica schist ores. The mica content of these ores are considerably higher than the pegmatites and alaskite ores now being mined, often containing in excess of forty percent mica. This-higher grade mica feed should promote a lower mining and milling cost with its resulting competative advantage. With more rigid government

Jan 1, 1969

By Charles R. Simcoe

The stress-strain curves in the microyield region for various Fe-C solid solutions shown by Davies and Ku are typical examples of parabolic curves defined by the expression a = kEn 111 These data, when replotted on log-log coordinates, as shown in Fig. 9, exhibit three essentially parallel straight lines. It is apparent that carbon increases the flow stresses, but does not affect the exponent n. In other words, the only factor in Eq. [1] affected by in in carbon content is the constant k. As Eq. [1] is written k is the stress at a strain of 1.0. This is unsatisfactory for examining data in the microyield region. Therefore, the equation can be altered to the form: to permit the use of the authors&apos; microyield stress at a strain of 10-6 as k. Extrapolating the curves in Fig. 9 to a strain of 10-6 gives stress values of 2000, 3200, and 5400 psi for 0.008, 0.014, and 0.02 pct C, respectively. These values do not agree exactly with the authors&apos; measured values, but this will not affect the following discussion. The effect of carbon content on the slopes of the stress-strain curves shown in Fig. 2 of the paper by Davies and Ku can be analyzed by differentiating Eq. [2] with respect to strain. Thus: where n is always less than 1.0. Since n is essen- tially constant as a function of carbon content for the data under discussion, the slopes of the stress-strain curves depend only on k and E. If the slopes are examined at various selected Plastic strains. i.e., 10-6, 10-5, and so forth, it follows from Eq. [3] that the dif-ferent slopes for the different carbon contents depend only on the different values of ke=10-6. Thus, the larger ke=10-6, the steeper the linear stress-strain curve will rise with increasing plastic strain. This

Jan 1, 1969

A pyrite flotation concentrate assaying 0&#183;065 oz/ton gold was investigated to determine the mode of occurrence of the gold. Ftom cyanidation and acid leaching experiments it was concluded that O&#183; 02-0&#183; 03 oz/ton goldwas in solid solution in pyrite and the balance of the gold was finely dispersed as grains throughout the pyrite.Autoradiography and electron-probe examination of possible areas in briquetted concentrate did not detect any grains of gold. Neutron irradiation and gamma spectrometry confirmed on 100 mg samples the fire assays obtained on 1 assay ton samples.Oxidation to hematite and reduction to magnetite at 600&#176;C made practically the whole of the gold extractable by cyanide. This technique could be of major significance for gold ores which contain a substantial amount of &quot;refractory&quot; gold.

Jan 1, 1969

A great range of contacting equipment is used in solvent extraction. However, a tower filled with a regular packing offers many advantages in the direct extraction from slurries. A study was made of the flow of a dense slurry through a packed tower in which the continuous phase was kerosene. The grid type packing, which was preferentially wetted by the slurry, had slats inclined at an angle of 30¦, to the horizontal. On the sur- face of the slats there were uniformly spaced longitudinal indentat- ions. These were of a height slightly less than the film thickness and divided the slurry discharging from the bottom of the slats into a number of uniform streams. When slurry entered the tower it was distributed by means of a troughs and weirs type of distributor. Because of the relatively high slurry velocities that occur at the entry region, it was necess- ary to have the distributor and the first two grids above the solvent level. The interface at the bottom of the tower was located at the mid-point of the bottom grid, so that the slurry entered the interface as a continuous film across the full width of the slats. Using the above system, stable flow with low entrainment was achieved at slurry flow rates of 3.4 mis/cm/sec. This would be equivalent to a flow rate of 177 gallons per minute through a tower of cross-section 4 ft 4 in. by 4 ft 10 in., or 1200 tons per day of solids of specific gravity 2.6 when the pulp density was 65 per cent. Previous tests indicated that a total tower height of about 30 ft would be required for a recovery of better than 99 per cent.

Jan 1, 1969