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Geophysics - Copper Soil Anomalies in the Boundary District of British ColumbiaBy T. M. Allen, W. H. White
THE Greenwood-Grand Forks area of southern central British Columbia, known as the Boundary District, has a long history of mining exploration and production. At the turn of the century this was the premier copper mining camp in the British Empire, its total production amounting to some 20 million tons. Most of this ore came from the great Granby mines at Phoenix, but the Motherlode mine at Deadwood camp, 6 miles to the west, and several mines in Summit camp, 5 miles north of Phoenix, made important contributions. The large deposits were exhausted in 1918 and the district since has seen only desultory exploration and salvage operations. The orebodies are mineralized skarn zones in limestone members of a thick series of Upper Paleozoic sedimentary and volcanic strata. Chalcopyrite is the primary ore-mineral. Copper carbonates and silicates occur sparingly in outcrops, but the oxidized zone generally is very shallow. Much of the surface is mantled by glacial drift which in most places ranges in thickness from 2 to 15 ft. In some of the hanging valleys, however, the glacial drift may be as much as 100 ft thick and may assume drumlin-like forms. In 1951 an ambitious program aimed at the discovery of new orebodies and important extensions of abandoned deposits was launched by Attwood Copper Mines, Ltd. In this district so thoroughly searched by an earlier generation of prospectors, any orebody which had remained undiscovered must have little or no surface indication. Consequently, in addition to the basic detailed geological work, the program of exploration included magnetometer and self-potential surveys. Geological bets and geophysical anomalies were tested further, prior to diamond drilling, by a study of copper distribution in tree twigs and/or in the soil. The soil sampling and analytical methods used and some of the results seem of sufficient importance to warrant this paper. The authors had done some plant sampling in this and other districts, using the dithizone neutral-color-end-point method (Warren and Delavault, 1948, 1949; White, 1950),1-3 but they were unfamiliar with its soil application. Finally, after much experimenting in the field, they adopted the methods described here. These methods are not entirely original or defensible on theoretical grounds, but under field conditions of rapid sampling and analysis the results are reliable enough to be of use. Fig. 1, which shows the results of duplicate analyses of duplicate soil samples taken at 50-ft intervals across an anomalous zone, indicates the relative dependability both of the sampling and analytical methods. Sampling and Analytical Equipment A 2-ft piece of 1-in. solid drill steel, one end sharpened to a broad, conical point. The steel is marked at 1 ft from the point. A 2-ft piece of ½-in. black iron pipe, one end filed to a bevelled cutting edge. The pipe is marked at 1 ft 3 in. from the cutting end. A 3-lb hammer. A plastic or rubberized sheet about 18 in. square. Moisture-proof assay pulp envelopes. A 10-mesh seive made from window screen with the paint burnt off. A small assay spatula. A pan balance sensitive to 10 mg. Two ignition trays about 4 in. square, made of sheet iron turned up along the edges. A Coleman two-burner gasoline stove. An asbestos board about 5x8 in., used as a hot plate on the gasoline stove. A circular aluminum rack to hold 8 test tubes while refluxing (design of Almond and Morris). Pyrex Glassware Large refluxing test tubes, 25x200 mm, marked at 40 ml volume. Breakers, 20 ml. Pipettes, 1, 5, and 10-ml capacity. Graduate, 50 ml. Shaking cylinders, 100 ml, glass stoppers. Burette, 25 or 50-ml capacity, with holder. Chemical Supplies 1 N sulphuric acid. Hydroxylamine hydrochloride, solid crystals. Fisher Alkacid test paper. Copper standard solution. Dithizone standard solution 60 mg per liter. Water reasonably free of metals. Soil Sampling Method: The problem of how to take a soil sample is extremely crucial. The method outlined below, adopted after a number of tests, has the advantages of uniform pattern, uniform depth, and uniform size of sample. The area to be tested was marked off by chain and compass lines 100 ft apart, normal to the strike of possible ore deposits. Numbered stakes were set at 50-ft intervals along these lines and a soil sample was taken at each stake in the following manner. The drill steel was driven into the ground normal to the slope of the surface to the marked depth of 1 ft, moved slightly from side to side, then carefully withdrawn. The iron pipe was inserted to the bottom of this hole, tapped down to the marked depth of 1 ft 3 in. and withdrawn; the 3-in. soil plug in the
Jan 1, 1955
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Institute of Metals Division - Transformation of Gamma to Alpha ManganeseBy E. V. Potter
For a nurnber of years, it has been known that manganese made by electro-deposition under certain conditions is ductile while under other conditions it is very brittle. The ductile metal is gamma manganese normally stable only between 1100 and 1138°C1; the brittle metal is alpha manganese, stable up to 727OC. The ductile metal is not stable, but gradually changes to the brittle form; the time required to complete the transfornlation is about 20 days at room temperature. Other observations have indicated that the transformation is completed in 10 to 15 min. at about 125°C, while at — 10°C, no appreciable change occurs in 9 months. The properties of gainma and alpha Illanganese in the pure state are ordinarilj difficult to determine because the gamma structure cannot be retained by normal quenching procedures and alpha manganese is so brittle, it is difficult to obtain specimens free from flaws. In a recent investigation2 some properties of gamma and alpha manganese were determined by studying the ductile electrolytic metal and determining the changes in its properties as it transformed to the brittle alpha form. These investigations provided an excellent opportunity for following the progress of the transition and studying its mechanism. The results of a series of such investigations are reported in this paper. Procedure Various properties of manganese were determined starting with the metal in the original ductile gamma form and following the subsequent changes in its properties as the metal transformed to the brittle alpha form. These observations were made at various temperatures, the data providing information regartling the mechanism of the transformation as well as the effect of temperature 011 the transition rate. Structure and resistivity values gave the most significant results, so this paper is concerned primarily with them. The structure was studied microscopically as well as by X ray diffraction. The resistivity was determined on strips of the metal by measuring the potential drop across a given length of the specimen. Current was passed through the specimen by wires soldered to its ends, and the potential connections were made by wires looped around the specimen near its center. The current was determined by the potential drop across a standard resistor connected in series with the specimen, the potential drop being measured on a potentiometer. In the temperature range from room temperature to 100°C an ordinary drying oven was used to heat the specimen. This was entirely satisfactory except at 100°C, where the time required to heat the specimen was long compared to the transition time, making the initial section of the resistivity curve unsatisfactory. To overcome this limitation, at 100°C and higher a thermostatically controlled oil bath was used to heat the specimens. The block on which the specimen was mountetl was plunged into the hot oil at the start of each test. The heating time was thereby reduced from 5 min. to about 6 sec, and dependable resistivity values could be obtained through 160°C. At this point the whole transition, including the warm-up time for the specimen, required only about 20 sec and it was not considered worth while trying to extend the temperature range further. Aside from the heating problem, the problem of making a sufficient number of accurate resistivity determinations became more and more difficult as the temperature was raised. Using the manually operated potentiometer, 100°C was about as far as it was possible to go. At this temperature and above, a self-balancing photoelectric recording potentiometer was used. Its response was quite rapid, and it proved to be entirely satisfactory all the way through 160°C, where the tests were stopped because of the specimen heating problem rather than any limitation of the potentiometer recorder. The metal used in these tests was prepared at the Salt Lake City laboratory of the Bureau of Mines. The method of preparation is discussed in a paper by Schlain and Prater.3 The sheets were about 2 3/8 by 5 3/16 in. and varied from 10 to 16 mils in thickness. They could be cut readily into pieces suitable for the various tests. X ray and microstructure determinations were made on pieces about 1/8 to 1/4 in. wide and about 1 in. long, while resistivity measurements were made on strips as long as possible and about 55 in. wide. The thickness of each sheet was not uniform over all its surface. This had no bearing on the X ray and microstructure determinations, but sections as nearly uniform and free from flaws as possible were chosen for the resistivity determinations. The gamma manganese was electro-deposited at 30°C, the time of deposition ranging from 5 to 12 hr for each sheet. Whenever possible, the tests were started directly after the metal was stripped from the cathode; otherwise the sheet was placed immediately
Jan 1, 1950
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Iron and Steel Division - Stabilization of Certain Ti2Ni-Type Phases by OxygenBy M. V. Nevitt
In the systems Ti-Mn-O, Ti-Fe-O, Ti-Co-O, and Ti-Ni-O the bounda.r-ies of the Ti2Ni-type phases were determined at one or more temperatures and the variation of the lattice parameter with oxygen content was determined. Densities were calculated from the lattice parameters and compared with measured density values. The: results indicate that the occurrence of the phase in these systesms can be correlated qualitatively with valency electron concentration, and that the role of oxygen is that of an electron acceptor. The lower limit of oxygen solubility appears to be determined by the valencies of Mn, Fe, Co, and Ni, while the maximum oxygen concentration coincides with the filling of the 16 (c) positions of the O 7h - Fd 3m space group. THE suggestion has been made by several investigators'" that the phases having the cubic E9,-type structure, and known as 17-carbide-type, double-carbide-type and Ti,Ni-type, are members of a family of electron compounds. This concept has been given additional support by recent work8 in which new isostructural phases involving second and third long period combinations were found, and which provided further evidence of the regularity of occurrence of the phase in terms of periodic table relationships. In this laboratory attention has been focused on the isomorphs containing titanium, zirconium, or hafnium, and the role that oxygen plays in their occurrence. In some binary systems Ti,Nitype* phases occur having the formula A,B where A is the titanium group element. Based on previous workq and the present investigation, oxygen is known to be soluble in two of these binary phases, Ti,Co and Ti2Ni. It is probable that oxygen is also soluble in the other phases of this kind. In other binary systems the Ti,Ni-type phase does not occur, but does occur in the corresponding ternary systems with oxygen .3-5 The experiments described here were performed to determine whether the occurrence and composition of certain of the Ti,Ni-type phases could be related to an electronic effect and whether oxygen's stabilizing role is exerted through an influence on the electron: atom ratio. The ternary systems Ti-Mn-O, Ti-Fe-O, n-Co-O, and Ti-Ni-O were selected for study for two reasons: First, several schemes have been proposed for first long period elements which, although not in quantitative agreement, show a generally consistent trend for the variation of valency with atomic number. Although for a transition metal the term valency is difficult to define and is generally not a constant number which can be applied to all alloys, it is usually assumed to be an index of the number of electrons per atom involved in metallic cohesion. Second, the determination of the Ti2Ni-type phase boundaries was facilitated by the fact that the phase relations in several of these ternary systems have been investigated by other workers."' EXPERIMENTAL PROCEDURE___________________ The alloys were prepared by arc melting crystal-bar titanium, reagent grade TiO, and electrolytic manganese, iron, cobalt, and nickel. Each button was remelted at least three times. The metals had a minimum purity of 99.9 pct except the nickel whose purity was 99.4 pct, the major impurity in this instance being cobalt. The preparation of the manganese alloys was attended by the customary difficulties associated with the vaporization of manganese. The technique used in this case was to add approximately 10 pct extra manganese to the original charge and to continue remelting the button until the final weight was in agreement with its intended weight. At least three alloys in each system were analyzed chemically and the results, even for the manganese alloys, were in good agreement with the intended compositions. A few additional alloys in the Ti-Mn-O system were prepared by the sintering of mixed powders in evacuated quartz tubes followed in some cases by arc melting. For annealing, the alloys were wrapped in molybdenum foil and placed in fused silica tubes containing zirconium chips. The fused silica tubes were evacuated at room temperature to a pressure of 1 x l0-6 mm of Hg and sealed. These capsules were then annealed for 72 hr at an external pressure of 5 x 10-5 mm of Hg in a vacuum furnace whose temperature could be controlled to + 1°C. The success of this procedure in avoiding significant oxygen or nitrogen pickup was indicated by the bright, ductile condition of the molybdenum foil and by the complete absence of a microscopic reaction layer on the specimens. This method did not permit rapid quenching of the specimens but in no case did metal-lographic examination indicate that a solid-state transformation had occurred on cooling. Metallo-
Jan 1, 1961
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Institute of Metals Division - Rate of Self-Diffusion in Polycrystalline MagnesiumBy P. G. Shewmon, F. N. Rhines
THE determination of the self-diffusion coefficient of magnesium has been made possible recently by discovery1-1 of a radioactive isotope, Mg28 having a half-life of 21.3 hr,1 and subject to manufacture in useful quantity. In the present research this material was condensed from the vapor phase upon a surface of high purity magnesium. The progress of diffusion of the tracer atoms into polycrystalline magnesium was followed by machining layers and measuring the change in the intensity of radiation as a function of the distance of each layer from the surface. The self-diffusion coefficient was found to be 2.1 X 10-8 sq cm per sec at 627°C, 3.6 X 10-9 sq cm per sec at 551°C, and 4.4 X 10-10sq cm per sec at 468°C; the activation energy is about 32,000 cal per mol. Experimental Procedure Since there was no other published measurement of a diffusion velocity in any magnesium-base material, is was necessary to employ a number of new experimental techniques. The short half-life of Mg28 made it necessary to complete the entire experimental procedure within three or four days. This meant that the work had to be done where a cyclotron was readily accessible and that all operations, prior to the diffusion heat treatment, had to be so designed as to minimize their time requirements. Unusual problems were imposed also by the chemical reactivity of magnesium, its high vapor pressure, and the fact that no satisfactory method for elec-trodepositing magnesium on magnesium is presently available. Finally, the machining and handling of the easily air-borne radioactive-magnesium chips involved certain health hazards, resulting in the need for further experimental restrictions. Preparation of Mg28 The Mg28 was produced in the Carnegie Institute of Technology syncrocyclotron by the neutron spallation of chlorine.5 his involved bombarding a 2 gram crystal of high purity NaCl with a beam of 350 mev protons for a period of 2 hr, after which the crystal was dissolved in warm water and the Mg28 was concentrated and purified by chemical means (see Appendix). About 50 microcuries of Mg28 thus were obtained in the form of magnesium oxinate (8 hydroxyquin-olatc?), which was ignited in air to produce MgO. This in turn was reduced to magnesium metal vapor, by the method of Russell, Taylor, and Cooper," in the vacuum apparatus shown schematically in Fig. 1. Here the essential part is a tantalum ribbon, slightly dished to receive the MgO. The ribbon, pre- viously outgassed at high temperature, is heated to about 1700°C by passing an electric current through it, whereupon tantalum oxide is formed, magnesium vapor is released almost instantaneously, and condensed partly upon the diffusion sample. Diffusion-Sample Preparation: Hot-extruded magnesium rod, 21/32 in. round was used in making the diffusion specimens. The magnesium analyzed as follows: 0.004 pct Al, 0.027 pct Fe, 0.040 pct Mn, 0.0004 pct Cu, 0.0002 pct Ni, and less than 0.01 pct Ca, 0.0004 pct Pb, 0.0011 pct Si, 0.001 pct Sn, and 0.001 pct Zn. A brief study of the crystal texture of this material revealed a sharp fiber texture with the (001) plane roughly parallel to the extrusion axis. Cylindrical samples 1/2 in. long by 5/8 in. were machined from this rod, the end faces dressed on 3/0 emery, and lightly etched with 20 pct HC1 in water. These samples then were annealed for at least twice the intended time of diffusion, at the intended diffusion temperature, in order to stabilize the grain structure at about 1 mm average diameter. The annealing treatments were conducted in argon in the same apparatus and in the same manner as the subsequent diffusion treatments, which will be described presently. Thus, a strain-free plane surface was produced, but there remained a layer of MgO which had largely to be removed before the layer of Mg28 was deposited. Most of this layer was taken off by two light passes over 3/0 emery paper. The balance of the oxide and a thin layer of metal were then removed by etching 5 to 10 min in 4 pct nital (4 pct HNO3 and 96 pct ethyl alcohol) made with absolute alcohol. There followed immediately three quick rinses in: 1-49 1/2 pct methanol, 49 1/2 pct acetone, and 1 pct formic acid, 2-50 pct methanol and 50 pct acetone, and 3-pure benzene. This procedure is essentially that of Sturkey.7 The resulting surface, which was of almost elec-tropolished brightness, remained plane and was free of cold work. It could be kept clean by storing under benzene, or in a desiccator; short exposure
Jan 1, 1955
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Institute of Metals Division - Structural Transformations in a Ag-50 At. Pct Zn AlloyBy T. B. Massalski, H. W. King
An hcp phase may be induced by cold working the ß' phase of the Ag-Zn system. This phase reverts to ß' on subsequent aging. No phase change occurs on cold working the o phase, but ß' is formed when the deformed alloy is subsequently aged at room temperature. It is concluded that for alloys near 50 at pct Zn the ordered bcc ß' phase is the equilibrium structure at room temperature. WhEN the disordered bcc ß phase of the Ag-Zn system is cooled to temperatures below 258o to 274oC, it transforms to a complex hexagonal phase <o.1,2 The nature of the o ß=o transformation has been the subject of some discussion,2'3 and the structure of o has been described in detail.' The latter phase appears to be stable on aging at room temperature but decomposes following cold work. When alloys containing approximately 50 at. pct Zn are rapidly quenched from the 0 phase field, the ß ? o transformation may be suppressed; but the ß phase undergoes an ordering reaction (ß ? ß'). The ß' structure may also be obtained as a result of cold working and aging at room temperature.4 Kitchingman, Hall, and Buckley4 have suggested that the decomposition of (o following cold work proceeds in two stages, (o ? ß followed by ß ? ß', but did not confirm this by experiment. When the ordered ' phases in the systems Cu-Zn5 and Ag-Cd6 are cold worked, they become unstable and transform to a close-packed hexagonal phase (( ) indicating that when order is destroyed in a ß' structure the close-packed hexagonal phase may in many cases be more stable. It thus became of interest to study more closely the effect of cold work and annealing on the stability of both the ß' and o phases in a Ag-50 at. pct Zn alloy. Predetermined weights of spectroscopically-pure Ag and Zn, supplied by Johnson and Matthey, were melted and cast under 1/2 atm of He in transparent vycor tubing. The ingot was homogenized for 1 week at 630°C and quenched into iced brine. Since mechanical polishing was found to induce a phase change, sections were first polished at room temperature, sealed in tubes under 1/2 atm of He, reannealed for several days at 630o or 200°C and then quenched into iced brine. Sections of the alloy thus prepared were found to be homogeneous when examined under the microscope. The sample quenched from 630°C (ß -phase region) was pink in color, whereas the sample quenched from 200°C (o-phase region) was silver. The latter sample showed the characteristic hexagonal anisotropy when examined under polarized light. Filings of the alloy were examined at room temperature, after various heat treatments, using an RCA-Siemens Crystalloflex IV diffractometer with filtered CuKa radiation. The X-ray reflections from flat powder specimens quenched from 630o and 200°C and sieved through 230 mesh were recorded graphically at a scanning speed of 1/2 deg per min. The resultant patterns are shown in Figs. 1(a) and 1(b) and may be identified as those of the 8' and <02 structures respectively. The lattice parameter of the ß' phase was determined as 3.1566Å.* This value compares very well withthatto be expected for a 50 at. pct Zn alloy from the data of Owen and Edmunds? and indicates that no loss of Zn occurred during casting. In order to study the effect of cold work upon the ß' and o phases, filings made at room temperature and sieved through 230 mesh were mounted immediately in the diffractometer-i.e., without a strain-relief anneal. Changes in structure on subsequent aging were followed by scanning repeatedly over the regions of the low index reflections of the ß' and o structures-i.e. , 28 from 35 to 44 deg. Immediately after filing the 8' specimen, additional diffraction peaks were observed in the low-index region of the pattern, as shown in Fig. 1(c). These additional peaks do not coincide with those of the o structure, Fig. l(b), but may be indexed as the (10.0), (00.2), and (10.1) reflections of an hcp phase (<) with nearly ideal axial ratio. However, this hexagonal phase appears to be very unstable since within a very short time at room temperature it reverts back to the ordered ß' phase, the reversion being complete within seven hours. The 5 ? ß' reversion reaction is, therefore, very similar to those already reported in Cu-Zn5 and Ag-Cd6 7'alloys. The action of filing caused the deformed surface of the originally pink ingot to become silver in color, indi-cating that the ( phase possesses similar reflecting properties to the o phase. Hence, the subsequent
Jan 1, 1962
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Thermal Metamorphism and Ground Water Alteration Of Coking Coal Near Paonia, ColoradoBy Vard H. Johnson
IN 1943 the U. S. Bureau of Mines undertook drilling in an effort to develop new reserves of coking coal in an area near Paonia, Colo., as a part of an attempt to alleviate the shortage of known coking coal of good quality in the western United States. Geologic mapping of the area was undertaken by the U. S. Geological Survey with the purpose of first furnishing guidance in location of drillholes and later aiding in interpreting the results of the drilling. The drilling program was under the general supervision of A. L. Toenges of the U. S. Bureau of Mines. J. J. Dowd and R. G. Travis were in charge of-the work in the field. Geologic mapping was started by D. A. Andrews of the Geological Survey in the summer of 1943 and was continued from the spring of 1944 to 1949 by the writer. The first few holes drilled failed to locate coking coal, but in the summer of 1944 coking coal was discovered by drilling 6 miles east of Somerset, Colo., the site of present mining. In the succeeding years, 1945 to 1948, 100 to 150 million tons of coal suitable for coking were blocked out by drilling. The ensuing discussion of the geologic controls on the distribution of coking coal in the area is based on the geologic mapping as well as the drilling done in the Paonia area, more complete descriptions of which have appeared or are in process of publication.1-5 In order that the possible geologic controls affecting the present distribution of coking coal may be considered, it is necessary to discuss briefly the indicators. of coking quality coals. Coking Coal Coal that cokes has the property of softening to form a pastelike mass at high temperatures under reducing conditions in the coke oven. This softening is accompanied by the release of the volatile constituents as bubbles of gas. After release of the contained gases and upon cooling, a hard gray coherent but spongelike mass remains that is referred to as coke. This substance varies greatly in physical properties and, to be suitable for industrial use, must be sufficiently dense and strong to withstand the crushing pressure of heavy furnace loads. Western coals have a generally high volatile content and therefore form a satisfactory coke only when they attain a rather high fluidity during the process of heating and distillation in-the coke oven. When this high degree of fluidity is developed, the volatile constituents escape and leave a finely porous coke. On the other hand, when the degree of fluidity is low the product is an excessively porous and therefore physically weak mass that is called char.6 Small quantities of oxygen present in coal are believed to decrease the fluidity of the material during the coking process and to favor the development of char rather than coke. In consequence, coal chemists have for some time considered the possibility of developing an index to coking. qualities by inspection of chemical analyses of coals.7 A formula has now been developed that does permit a rough preliminary estimate of the cokability of coal on the basis of the analysis on an ash and moisture-free basis. Coals may be eliminated as possible coking fuels if the oxygen content is greater than 11 pct. Similarly the ratio of hydrogen to oxygen must be greater than 0.5 and the ratio of fixed carbon to volatile constituents must be greater than 1.3. If the coal, on the basis of these limiting factors, appears to have possible coking qualities, the following formula permits determination of the coking index: Coking index =[ a+b+c+d 5] a equals 22/oxygen content on ash and moisture- free basis, . b equals two times the hydrogen content divided by oxygen content on moisture and ash-free basis, c equals fixed carbon/1.3 x volatile matter, and d equals the heating value on moist, ash-free basis/13,600. Coking indices higher than 1.0 suggest that the coal will coke, and indices above 1.1 indicate good coking tendencies. Although generally usable, this formula is not completely satisfactory because the percentage of oxygen shown in ultimate analyses is derived only by difference; i.e., by subtracting the sum of the percentages of the constituents determined analytically from 100 pct.8,9 Although the coking index indicates the coking tendencies of coal, it is necessary to make physical tests of coke before its industrial value can be determined. The U. S. Bureau of Mines has developed a standard procedure for determining the approximate strength of coke that would be formed from a given coal. In this test one part of ground coal, mixed with 15 parts of carborundum, is baked to form a standard briquette. The weight, in kilograms, necessary to crush the briquette is termed the agglutinating index. This test determines the relative fluidity attained in the coking process by measuring the cementing strength of the coal in the briquette. A
Jan 1, 1952
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Reservoir Engineering - Variable Characteristics of the Oil in the Tensleep Sandstone Reservoir, Elk Basin Field, Wyoming and MontanaBy Joseph Fry, Ralph H. Espach
In the spring of 1943, when it was evident that the Tensleep bandstone in the Elk Basin Field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes. of gas in solution. saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep Reservoir of the Elk Basin Field has unusually varying physiral characteristics, such as a saturation pressure of 1,250 psia and 490 cu ft of gas in solultion in a barrel of oil at the crest of the structure and a saturation pressure of 530 psia and 134 cu ft of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the gas in solution in the oil varies from 18 per cent for oil on the crest to 5 per cent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of the oil in the structure. Many geologists and petroleum engineers have considered that all the oil in a petroleum reservoir has rather uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas; that such is not always so is borne out by the results of the study by the writers. INTRODUCTION The Rocky Mountain region is one in which may be found striking examples of the unusual in oil and gas accumulations, as is evident from the following: The high helium content (7.6 per cent) of the gas in the Ouray-Leadville limestone sequence in the Rattlesnake Field, New Mexico, and gases of similar helium content in other fields; 50" to 55' API gravity distillate in solution in carbon dioxide gas and recoverable through retrograde condensation, in the North McCallum Field, Colorado; the occurrence of gas, oil, or both in closely related structures contrary to the usual concepts of gravimetric segregation: the accumulation of gas and/or oil in structures closely related to other structures that apparently are more favorable but do not contain oil or gas accumulations; the high hydrogen sulfide content (as high as 42 per cent) of the gas associated with oil in some fields in the Big Horn Basin, Wyoming; and the wide range of fluid chararteristics found in the Elk Basin reservoir. Elk Basin, an interesting old oil field that has been producing oil from the Frontier formation since 1915, is situated in a highly eroded basin resulting from the erosion of the crest of an anticline and some of the underlying softer shales. The field came back into national prominence during 1943 when it became known that it was the largest single reserve of new oil discovered in the United States that year. The Tensleep sandstone was found to contain oil in November. 1942, when a well drilled to a depth of 4,538 ft (44 ft into the Tensleep sandstone) flowed oil at the rate of 2,500 B/D. By the end of 1949, 137 oil-producing wells and five dry holes had been drilled, and approximately 32 million bbl of oil had been produced. Approximately 6,000 acres may be considered productive of oil in the Tensleep Reservoir, and estimates of the oil that will be produced average 200 million bbl. The Tensleep Reservoir has further interest because it ha-greater closure than any oil field in the Rocky Mountain region; the closure of the Elk Basin anticline is variously estimated at 5.000 to 10,000 ft. of which the top 2.00 ft of the structure contained oil. SUBSURFACE OIL SAMPLING Fig. 1 is a structural map of the Elk Basin Tensleep Reservoir, on which the nine wells used in this study and the numbers correvponding to the well designations hereafter referred to are shown. Wells 1. 2, 3, 4, and 8 were tested and sampled during October and November. 1943. and Wells 5, 6. 7, and 9 during June and July, 1944. An electromagnetic type sampler developed by the Bureau of Mines and described by Grandone and Cook' was used in obtaining the subsurface oil samples. As the wells were tubed nearly to bottom, the sampler was run as far as possible in the tubing hut never below the top perforations. The following procedure was used in testing and sampling the wells: A well was shut in for at least three days, after
Jan 1, 1951
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Reservoir Engineering - Variable Characteristics of the Oil in the Tensleep Sandstone Reservoir, Elk Basin Field, Wyoming and MontanaBy Joseph Fry, Ralph H. Espach
In the spring of 1943, when it was evident that the Tensleep bandstone in the Elk Basin Field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes. of gas in solution. saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep Reservoir of the Elk Basin Field has unusually varying physiral characteristics, such as a saturation pressure of 1,250 psia and 490 cu ft of gas in solultion in a barrel of oil at the crest of the structure and a saturation pressure of 530 psia and 134 cu ft of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the gas in solution in the oil varies from 18 per cent for oil on the crest to 5 per cent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of the oil in the structure. Many geologists and petroleum engineers have considered that all the oil in a petroleum reservoir has rather uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas; that such is not always so is borne out by the results of the study by the writers. INTRODUCTION The Rocky Mountain region is one in which may be found striking examples of the unusual in oil and gas accumulations, as is evident from the following: The high helium content (7.6 per cent) of the gas in the Ouray-Leadville limestone sequence in the Rattlesnake Field, New Mexico, and gases of similar helium content in other fields; 50" to 55' API gravity distillate in solution in carbon dioxide gas and recoverable through retrograde condensation, in the North McCallum Field, Colorado; the occurrence of gas, oil, or both in closely related structures contrary to the usual concepts of gravimetric segregation: the accumulation of gas and/or oil in structures closely related to other structures that apparently are more favorable but do not contain oil or gas accumulations; the high hydrogen sulfide content (as high as 42 per cent) of the gas associated with oil in some fields in the Big Horn Basin, Wyoming; and the wide range of fluid chararteristics found in the Elk Basin reservoir. Elk Basin, an interesting old oil field that has been producing oil from the Frontier formation since 1915, is situated in a highly eroded basin resulting from the erosion of the crest of an anticline and some of the underlying softer shales. The field came back into national prominence during 1943 when it became known that it was the largest single reserve of new oil discovered in the United States that year. The Tensleep sandstone was found to contain oil in November. 1942, when a well drilled to a depth of 4,538 ft (44 ft into the Tensleep sandstone) flowed oil at the rate of 2,500 B/D. By the end of 1949, 137 oil-producing wells and five dry holes had been drilled, and approximately 32 million bbl of oil had been produced. Approximately 6,000 acres may be considered productive of oil in the Tensleep Reservoir, and estimates of the oil that will be produced average 200 million bbl. The Tensleep Reservoir has further interest because it ha-greater closure than any oil field in the Rocky Mountain region; the closure of the Elk Basin anticline is variously estimated at 5.000 to 10,000 ft. of which the top 2.00 ft of the structure contained oil. SUBSURFACE OIL SAMPLING Fig. 1 is a structural map of the Elk Basin Tensleep Reservoir, on which the nine wells used in this study and the numbers correvponding to the well designations hereafter referred to are shown. Wells 1. 2, 3, 4, and 8 were tested and sampled during October and November. 1943. and Wells 5, 6. 7, and 9 during June and July, 1944. An electromagnetic type sampler developed by the Bureau of Mines and described by Grandone and Cook' was used in obtaining the subsurface oil samples. As the wells were tubed nearly to bottom, the sampler was run as far as possible in the tubing hut never below the top perforations. The following procedure was used in testing and sampling the wells: A well was shut in for at least three days, after
Jan 1, 1951
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Iron and Steel Division - Relation between Chromium and Carbon in Chromium Steel RefiningBy D. C. Hilty
It has long been known that in melting high-chromium steels, some of the carbon might be oxidized out of the melt without excessive simultaneous oxidation of chromium, and that higher temperatures favor retention of chromium. The advent of oxygen injection as a tool for rapid decarburization of a steel bath permits significantly higher bath temperatures, and it was quickly recognized that the use of oxygen injection facilitated the oxidation of carbon to low levels in the presence of relatively high residual chromium contents. Up to the present time, however, specific data pertaining to the chro-mium-carbon-temperature relations in chromium steel refining have not been available. Individual steelmakers have evolved practices more or less empirically, but there has been very little real basis for predicting how effective any given practice can be in permitting maximum oxidation of carbon with minimum loss of chromium. The current investigation, therefore, was undertaken in an effort to establish the fundamental carbon-chromium relationship in molten iron under oxidizing conditions. As reported below, the equilibrium constant and the influence of temperature on that constant have been derived for the iron-chromium-carbon-oxygen reaction in the range of chromium steel compositions with what appears to be a fair degree of precision. The practical application of the result will be obvious. Experimental Procedure The laboratory investigation was carried out on chromium steel heats melted in a magnesia crucible in a 100-lb capacity induction furnace at the Union Carbide and Carbon Re- search Laboratories. The charges for the heats consisted of Armco iron, low-carbon chromium metal, and high-carbon chromium metal, the relative proportions of which were calculated so that the various heats would contain from approximately 0.06 pct carbon and 8 pct chromium to 0.40 pct carbon and 30 pct chromium at melt-down. When the charges were melted, the bath temperatures were raised to the desired level, and the heats were then decarburized by successive injections of oxygen at the slag-metal interface through a ½-in. diam silica tube at a pressure of 30 psi. The duration of the oxygen injections was from 30 sec to 2 min. at intervals of approximately 5 to 30 min. It did not appear that length or frequency of the injection periods had any significant effect on the results; cansequently, no effort was made to hold them constant and they were controlled only as was expedient to the general working of the heats. Between successive injections, the heats were sampled by means of a copper suction-tube sampler that yields a sound, rapidly-solidified sample representative of the composition of the molten metal at the temperature of sampling. This sampling device is a modification of the one described by Taylor and Chipman.1 An attempt was made to vary bath temperatures between samples, but it quickly became evident that, unless the variations were small or unless the new temperature was maintained for a minimum of 15 min. during which an injection of oxygen was made in order to accelerate the reactions, a very wide departure from equilibrium resulted. For most of the runs, therefore, temperature was maintained relatively constant at approximately 1750 or 1820°C. A few reliable observations at other temperatures, however, were obtained. Temperature Measurement The high temperatures involved in this investigation were measured by the radiation method, utilizing a Ray-O-Tube focused on the closed end of a refractory tube immersed in the metal bath. The immersion tubes employed were high-purity alumina tubes specially prepared by the Tona-wanda Laboratory of The Linde Air Products Co. These tubes were quite sturdy under reasonable mechanical stress at high temperature. They were unusually resistant to thermal shock, and chemical attack on them by the melts was slow. With care, it was found possible to keep these tubes continuously immersed in a heat for as long as 5 hr at temperatures up to 1850°C, before failure by fluxing occurred. The Ray-O-Tube—alumina tube assemblage was similar to those supplied commercially for lower temperature applications. In operation, the alumina tube was slowly immersed in the molten metal to a depth of approximately 5 in., and the device was then clamped solidly to a supporting jig where it remained for the duration of the run. A photograph of the equipment, in operation with Ray-O-Tube in place and oxygen injection in progress, is shown in Fig 1. When in position in a heat, the instrument was calibrated by means of an immersion thermocouple and an optical pyrometer. For calibration through the range of temperatures from 1500 to 1650°C, a platinum -platinum + 10 pct rhodium thermocouple in a silica tube was immersed alongside the alumina tube. Output of the Ray-O-Tube in millivolts and the
Jan 1, 1950
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Block Cave Mining at the Mather MineBy Paul R. Bluekamp
The Mather Mine property is composed of a 5.2 sq km (2 sq mile) area within the Cities of Ishpeming and Negaunee which are located in the Upper Peninsula of Michigan. Production in this mine started in 1943; it ran continuously until its closing in 1979, having produced slightly over 55 million tons of iron ore. This mine was a joint venture between several steel companies and The Cleveland- Cliffs Iron Company (CCI), with CCI being the fee holder and operator. For the first 17 years of operation, the ore was shipped in its natural state directly from the mine to the steel mill. By 1960, iron ore pellets were on the market and they proved so superior to the natural soft Mather ore that the latter became difficult to sell except for the coarser portions. It was decided to develop a pelletizing process for the Mather ore, and this was accomplished by 1965 when the first Mather pellets were produced. From this date, all but the coarse fraction of the Mather ore was shipped as pellets. The geological setting is that of a large east-west trending synclinorium which plunges to the west. The lowest member of this trough-like structure is, for the most part, a quartzite-like graywacke, the upper 20 m of which grades into a softer, fine grained slate. Lying conformably on this graywacke footwall member is an iron- formation member which is over 1,300 m in thickness. This iron-formation is cow posed of thin alternate bands of iron oxides and chert and is intruded by a number of diorite sills - some up to 122 rn (400 ft) in thickness. The north limb of this synclinorium dips at approximately 45' and bottoms out at about 1,000 m from surface in the central part of the mine. There are two sets of faults, many of which are intruded by diorite dikes, which trend east-west and southeast-northwest. Displacements are varied, reaching a maximum displacement of 243 m (800 ft). The ore is found lying directly on the slatey footwall and its position is largely controlled by the faults and dikes, with the bulk of the ore being on the upper side of these structures. The ore is composed of soft earthy hematite and martite with vertical thicknesses up to 122 m (400 ft) although the average thickness would be closer to 46 m (150 ft). The ore averaged 60% iron and 7% silica on a dried analysis. The Mather Mine is located on the north limb of the syncline and was worked from two shafts, the deepest of which. was 1,09 7 m. These two shafts are about 2 km apart and serviced a total of 8 working levels between them during the life of the mine. The level spacing was about 61 m (200 ft). The main haulageways were driven parallel to the ore/footwall contact in the hard cow petent graywacke wherever possible. On the lower levels, deeper into the footwall, naked development was common. This material graded into roof bolting ground towards the upper stratigraphic portion. As drifting progressed further into the upper stratigraphic portion of the footwall, progressively stronger steel sets had to be used. From the main haulageway, cross-cuts were turned into the orebody on 61 m (200 ft) centers and extended as far as needed to recover the ore available to that particular cross-cut. The main haulageways and cross-cuts were driven 3 m (10 ft) high, 3 m (10 ft) wide at the top and 4.6 m (15 ft) wide at the bottom. This configuration would accomodate a set composed of a 2.7 m (9 ft) cap on top of two 2.7 m (9 ft) legs angled out at 18'. A sill plate was used under each leg to prevent its sinking into the ore below. The type of steel used was dependent on the expected weight to be experienced. Sets were placed on 1.63 m (5 ft 4 in.) centers; however, in extremely heavy areas, it was sometimes necessary to install sets on 0.8 m (2 ft 8 in.) centers. On the top two levels (5th and 6th), the ore was considerably hard-er and was mined by sub-level stoping and long hole drilling. Very light steel sets were used in the main haulageways and cross-cuts and timber was used in the production drifts. Some con- crete production drifts were installed on 6th level, but proved to be uneconomical. However, as mining reached greater depths, the ore became softer and more massive, reaching its maximum vertical heights on 11th and 12th levels. On levels 7 through 10, yielding steel sets were used extensively in the slusher drifts. While they were satisfactory on 7th and 8th levels, their success diminished with depth and they were
Jan 1, 1981
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Geophysics - Geophysical Case History of a Commercial Gravel DepositBy Rollyn P. Jacobson
THE town of Pacific, in Jefferson County, Mo., is 127 miles west of St. Louis. Since the area lies entirely on the flood plain of a cutoff meander of the Meramac River, it was considered a likely environment for accumulation of commercial quantities of sand and gravel. Excellent transportation facilities are afforded by two major railways to St. Louis, and ample water supply for washing and separation is assured by the proximity of the river. As a large washing and separation plant was planned, the property was evaluated in detail to justify the high initial expenditure. An intensive testing program using both geophysical and drilling methods was designed and carried out. The prospect was surveyed topographically and a 200-ft grid staked on which electrical resistivity depth profiles were observed at 130 points. The Wenner 4-electrode configuration and earth resistivity apparatus" were used. In all but a few cases, the electrode spacing, A, was increased in increments of 11/2 ft to a spread of 30 ft and in increments of 3 ft thereafter. Initial drilling was done with a rig designated as the California Earth Boring Machine, which uses a bucket-shaped bit and produces a hole 3 ft in diam. Because of excessive water conditions and lack of consolidation in the gravel there was considerable loss of hole with this type of equipment. A standard churn drill was employed, therefore, to penetrate to bedrock. Eighteen bucket-drill holes and eight churn-drill holes were drilled at widely scattered locations on the grill. The depth to bedrock and the configuration will not be discussed, as this parameter is not the primary concern. Thickness of overburden overlying the gravel beds or lenses became the important economic criterion of the prospect.** The wide variety and gradational character of the geologic conditions prevailing in this area are illustrated by sample sections on Fig. 2. Depth profiles at stations E-3 and J-7 are very similar in shape and numerical range, but as shown by drilling, they are measures of very different geologic sequences. At 5-7 the gravel is overlain by 15 ft of overburden, but at E-3 bedrock is overlain by about 5 ft of soil and mantle. Stations L-8 and H-18 are representative of areas where gravel lies within 10 ft of surface. In most profiles of this type it was very difficult to locate the resistivity breaks denoting the overburden-gravel interface. In a number of cases, as shown by stations M-4 and H-18, the anomaly produced by the water table or the moisture line often obscured the anomaly due to gravel or was mistaken for it. In any case, the precise determination of depth to gravel was prevented by the gradual transition from sand to sandy gravel to gravel. In spite of these difficulties, errors involved in the interpretation were not greatly out of order. However, results indicated that the prospect was very nearly marginal from an economic point of view, and to justify expenditures for plant facilities a more precise evaluation was undertaken. The most favorable sections of the property were tested with hand augers. The original grid was followed. In all, 46 hand auger holes were drilled to gravel or refusal and the results made available to the writer for further analysis and interpretation. When data for this survey was studied, it immediately became apparent that a very definite correlation existed between the numerical value of the apparent resistivity at some constant depth and the thickness of the overburden. Such a correlation is seldom regarded in interpretation in more than a very qualitative way, except in the various theoretical methods developed by Hummel, Tagg (Ref. 1, pp. 136-139), Roman (Ref. 2, pp. 6-12), Rosenzweig (Ref. 3, pp. 408-417), and Wilcox (Ref. 4, pp. 36-46). Various statistical procedures were used to place this relationship on a quantitative basis. The large amount of drilling information available made such an approach feasible. The thickness of overburden was plotted against the apparent resistivity at a constant depth less than the depth of bedrock for the 65 stations where drilling information was available. A curve of best fit was drawn through these points and the equation of the curve determined. For this relationship the curve was found to be of the form p = b D where p is the apparent resistivity, D the thickness of overburden, and b a constant. The equation is of the power type and plots as a straight line on log-log paper. The statistical validity of this equation was analyzed by computation of a parameter called Pearson's correlation coefficient for several different depths of measurements, see Ref. 5, pp. 196-241. In all but those measurements taken at relatively shallow depths, the correlation as given by this general equation was found to have a high order of validity on the basis of statistical theory.
Jan 1, 1956
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Institute of Metals Division - The Role of Oxygen in Strain Aging of VanadiumBy O. N. Carlson, S. A. Bradford
Discontinuous yielding in tensile tests was observed in V-O alloys in the temperature ranges of 150° to 175°C and also 350° to 400°C. The magnitude and intensity of the serrations were found to vary considerably with oxygen content. Maxima were observed in tensile and yield strengths and in the strain-hardening coefficient at the higher temperature only. The strain rate sensitivity was observed to be negative between 150° and 400°C. THIS investigation was undertaken to study the effect of oxygen on the tensile properties of iodide vanadium in the temperature range of 25o to 450°C. Brown1 observed an increase in strength between room temperature and 400°C in vanadium metal, and found that oxygen and nitrogen had a rather pronounced effect on the strength and ductility. A maximum in the tensile strength was observed by Rostoker et al.2 near 300oC and by Pugh3 around 450°C for calcium-reduced vanadium. Pugh also found a maximum in the yield strength and in the strain-hardening exponent, and minima in the elongation and strain rate sensitivity at the same temperature. Eustice and Carlson4 reported the appearance of serrations in the stress-strain curves between 140° and 180°C in iodide vanadium containing 600 ppm O. These anomalies in the mechanical properties indicate that strain aging occurs in vanadium, but the impurity or impurities responsible for the above-mentioned effects have not been identified. The phenomenon of strain aging is usually characterized by the return of the yield point after interruption of a strength test. In the temperature range where strain aging occurs, the yield and tensile strengths attain maximum values, elongation and strain rate sensitivity exhibit minima, and discontinuous yielding is generally observed in the stress-strain curve. Cottrell5, 6 has postulated that strain aging is due to the migration of solute atoms to dislocation sites to produce locking after the dislocations have broken free from their impurity atmospheres during the initial yielding. At the strain-aging temperature the process is a dynamic one in which the solute impurity atoms diffuse to the vicinity of the moving disloca- tion producing "locking" which gives rise to maxima in the tensile strength and serrations in the elongation curves. Cottrel17 has noted that discontinuous yielding in iron occurs when the diffusion coefficient of nitrogen, D, and the strain rate, i, are related by D = 10-9 €. EXPERTMENTAL PROCEDURE The vanadium metal employed in this study was prepared by the iodide refining process as described by Carlson and owen.8 A representative analysis of the vanadium used in this investigation was: 150 ppm O, <5 ppm N, <1 ppm H, 150 ppm C, 150 ppm Fe, 70 ppm Cr, <50 ppm Si, 30ppm Cu, 20 ppm Ni, <20 ppm Ca, <20 ppm Mg and <20 ppm Ti. Alloys containing from 200 to 1800 ppm O, all of which lie in the solid solution range of the V-O system, were prepared by arc melting vanadium together with portions of a high-oxygen master alloy. The master alloy was prepared by tamping pure V2O5 into holes drilled in a vanadium ingot and arc melting this five or six times in an inert gas atmosphere, inverting the button between each melting step. The oxygen content of the master alloy was then determined by vacuum fusion analysis. Vanadium containing less than 150 ppm O was prepared in the following manner. A bar of iodide vanadium was deoxidized by sealing it in a tantalum crucible with a few grams of high-purity calcium. This was held at 1100°C for 4 days to allow time for the oxygen to diffuse to the surface and to react with the calcium vapors. The calcium oxide product was later dissolved from the surface of the bar with dilute acetic acid. In this way vanadium containing from 20 to 50 ppm O was prepared. Sample Preparation. The are-melted ingots were cold swaged into 3/16-in. diam rods and these were machined into cylindrical tensile specimens with a reduced section of 1.00-in. length and 0.120-in. diam. The test specimens were annealed for 4 hr at 900°C in a dynamic vacuum of mm of Hg to remove hydrogen from the metal. This recrystal-lization treatment produced a uniformly fine-grained structure with a mean grain size of approximately 0.06-mm diam. The oxygen contents reported in this paper were determined by a vacuum fusion analysis of the tensile specimens after testing. Analyses for other interstitial or metallic impurities showed no significant changes from that of the original material. Tension Tests. Tension tests were performed on a screw-driven tensile machine at a constant cross-head speed of 0.01 in. per min. Tests at elevated temperatures were carried out by heating the
Jan 1, 1962
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Institute of Metals Division - Contribution to the Metal-Carbon-Boron SystemsBy F. W. Glaser
Metal-carbon-boron powder mixtures were hot pressed and the resulting specimens were studied by X-ray diffraction. It was found that regardless of the starting combination of the metal, carbon, or boron powders, a metal boride phase was always the major component in these samples. In the absence of carbon the boride phase formed on hot pressing depended only on the amount of boron present. Two new phases of the system Ti-B were found. They are Ti2B and Ti2B5. The existence of a controversial face-centered cubic phase of formula TiB was confirmed. Electrical resistivities were measured for various boride phases. It was found that the diborides are generally better conductors than the monoborides of the same metal. THE carbides and borides of the transition elements have very high melting points, in the range 2500° to 4000°C, and are therefore of interest as high temperature materials. The literature on the stability or chemical reactivity of these carbides and borides is very scarce. Various investigators'-" have demonstrated a relative instability of certain carbide phases in the presence of boron or boron-containing substances. In a recent publication, Glaserl demonstrated the stability of zirconium-boride (ZrB,) in the presence of carbon at temperatures in excess of approximately 2900°C, while during a preliminary investigation of boride phases, Steinitz' concluded that the diborides are stable in the presence of carbon while the monoborides of the fourth and fifth group are not, forming diborides plus carbides instead. Nelson, Willmore, and Womeldorph" have elaborated on the reaction B,C + 2TiC = 2TiB, + 3C, which was known to occur because of a relative instability of B,C and the great tendency towards TiB, formation at relatively low temperatures (approximately 1200°C). A similar study, involving as starting materials TiO, and B,C and resulting in TiB,, was recently described by Honak4, who observed the beginning of an exothermic reaction of a Ti0,-B,C powder mixture, which, when preheated in a hydrogen atmosphere to approximately 950°C, was carried to about 1600 °C by the heat of reaction. To shed more light on reactions of this type (Metal-C-B), the final product apparently always resulting in a boride phase at the expense of a carbide phase," a systematic investigation was started * Boride phases of various metals, as reported to date, are listed in Table I. and the following is an account of some of the results that were obtained. Materials, Preparation of Samples, Testing Methods The raw materials employed for this work consisted of various carbide, boride, and metal powders. as well as of boron and graphite powders. In cases where commercial grades of carbides were considered unsuitable because of low purity or excessive amounts of graphitic carbon, such carbide powders were prepared by this laboratory. The procedure for the preparation of carbide powders (zirconium carbide, titanium carbide, tantalum carbide, and niobium carbide) consisted of mixing graphite and the respective metal hydride powders in stoichio-metric proportions and subsequent heating of such mixtures in a hydrogen atmosphere in carbon crucibles. The heating was by high frequency to temperatures ranging between 1700" and 2100°C. The resulting carbide was then comminuted and screened to the desired particle size. ZrB, and TiB, powders were produced by the electrolysis of fused salt baths, according to the method described by Andriex.. The borides of niobium, vanadium, tantalum, molybdenum, chro-ium, and iron were obtained by mixing the respective metal and boron powders in the desired proportions. Such metal-boron mixtures were heated in a high frequency furnace to form boride powders. For each metal-carbon-boron group (Tables I1 through XI) a metal, its hydride, carbide or boride were mixed with carbon, boron or boron carbide powders. The additions of carbon, boron or boron carbide powders to any of these metals or metal compounds were calculated to satisfy a particular carbide or boride phase that according to the literature (Table I) had definitely been established by X-ray diffraction work. Samples of powder mixtures were hot pressed in graphite molds that were heated by direct conduction. The specimen dimensions were approximately 2.5X1X1 cm. Hot pressing temperatures were measured optically and maintained for approximately 30 sec under a constant pressure of about 1.3 ton per sq in. Wherever possible, an attempt to obtain maximum specimen density was made by temperature variation. Electrical resistivity testing was done by measuring potentiometrically the voltage drop over a length of 1.5 cm for a current of 10 amp, at room temperature. To obtain electrical resistivities for specific carbide or boride phases, values were plotted as a function of the respective sample densities
Jan 1, 1953
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Discussion of Papers Published Prior to 1958 - Filtration and Control of Moisture Content on Taconite ConcentratesBy A. F. Henderson, C. F. Cornell, A. F. Dunyon, D. A. Dahlstrom
Ossi E. Palasvirta (Development Engineer, Oliver Iron Mining Diu., U. S. Steel Gorp.)—The authors are to be congratulated for their interesting article, which thoroughly illustrates the variables inherent in filtration of taconite concentrate. The work and the conclusions based thereon largely parallel the test work done by the writer at the Pilotac plant" and the experience gained with a commercial size agitating disk filter in the same plant. At Pilotac, however, a thorough study was also made of the effect of depolarizing (demagnetizing) the filter feed, and it is the purpose of this discussion to comment on the merits of depolarization of the magnetite concentrate prior to filtering. The work at Pilotac was done in three phases: 1) preliminary laboratory testing with a circular filter leaf of 0.047 sq ft, followed by 2) plant testing using a 4-ft diam, single-disk agitating filter that was purchased on the basis of the pilot tests on the 4-ft model. In the laboratory tests depolarization was achieved by slowly withdrawing' batches of thickened concentrate from a coil producing an alternating field of about 300 oersteds. In plant tests the standard Pilotac procedure' was employed, wherein the pulp falls freely through the depolarizing coil. The preliminary tests in the laboratory at first seemed to indicate that although depolarization of the filter feed decreases the cake moisture, it also tends to decrease the thickness of the cake, thus decreasing filtering rate. The tests with the 4-ft disk filter soon showed, however, that the compactness of the cake, attained during the form period because of depolarization, permitted a considerable decrease in drying time without any sacrifice in final moisture content. Thus, the filter could be operated at a much higher speed, and the overall capacity was higher than with magnetized feed. Because of the great compactness of the cake there was little shrinkage during the drying period, which prevented cracking and subsequent loss in vacuum. This in turn permitted operation with as thick a feed pulp as the diaphragm pumps could handle, eliminating the necessity of pulp density control. On the basis of these findings, the 6-ft agitating disk filter has been operated at 2 rpm, using feed pulps varying from 65 to 73 pct solids. Initially Saran 601 was used as medium, but it was later replaced with a relatively open, tight-twist nylon cloth. Filtering rates up to 750 lb per ft- er hr can be attained with feeds averaging about 70 pct- 270 mesh, and there is no trouble because of cracking. The cake moistures vary between 8.5 and 9.5 pct. To recapitulate, the merits of depolarizing the filter feed may be summed up as follows: 1) The well dispersed pulp shows less tendency to settle in the filter tank. 2) The homogeneous filter pool results in more even cake formation. 3) Because of absence of flocs, great compactness of cake is attained during the form period. 4) The cake does not tend to crack during the drying period. 5) A drier cake is produced. 6) A shorter drying period is necessary, permitting higher operating speed, which in turn results in increased capacity. 7) Density of the feed pulp can be kept as high as the equipment can handle. This increases capacity, since it is directly proportional to the percentage of solids in the pool. A few tests were also made to study the effect of chemical flocculants on filtration efficiency. Results showed that the effects of chemical and magnetic floc-culation were quite similar. Thus the use of a floccu-lant would impair rather than improve the filtering of magnetite concentrate. A. F. Henderson, C. F. Cornell, A. F. Dunyon and D. A. Dahlstrom (authors' reply)—We want to thank O. E. Palasvirta for his comments, particularly in view of the encouraging results obtained with demagnetized taconite concentrate. In our studies an attempt was made to evaluate the effects of depolarizing the feed to the plant filters by passing the slurry through a coil, similar to the method described by Palasvirta. Unfortunately, in our experiments there were no startling improvements in performance level, neither cake rate increase nor cake moisture reduction. However, when slow filter cycle speeds were employed, the filter cake tended to crack and the vacuum level dropped, resulting in an increase in cake moisture content. When demagnetized feed was used during slow speeds, no cake cracking was evidenced and the vacuum level remained constant. Thus the depolarizing coil was found necessary only in cases of cracking. It should be noted that most of our test work concerned a feed of 85 to 90 pct —335 mesh and about 60 pct by weight solids concentration. This contrasts with 70 pct —270 mesh and 65 to 73 pct by weight solids as noted by Palasvirta. Reviewing both sets of results, it might be concluded that depolarizing may be successfully employed to alleviate cake cracking tendencies and may markedly improve cake rates and moistures on the coarser taconite concentrates. Further investigations may disclose the exact relationship of grind and pulp density to the depolarizing action.
Jan 1, 1959
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Extractive Metallurgy Division - The Fume and Dust Problem in IndustryBy H. V. Welch
In this paper, as prepared for delivery at the Southern California regional meeting on Oct. 14, 1948, it was thought best to interpret the term "economics" in a rather broad manner and to include, in addition to the material losses and recoveries and associated monetary values (Part I), a limited discussion of the increased difficulties or the particular problem and the special requirements, as the particle sizes of the suspended particles range down from the relatively coarse to 100, to 10, to 1 micron or even to a fraction of one micron (Part II). Further, it is not quite in order to overlook entirely the community and individual health problems, although space requires the economics of this to be considered only very incompletely. Therefore, Part III, covering this phase of the subject, is very limited. This paper, then, is divided into 5 parts or headings as follows: I Losses and/or values in suspended solids. II Particle size. III Dust and fumes in community and individual living. IV Means and Procedures for dust and fume collection. V Description or examples of specific equipment in service and of the several types used for dust and fume collection. Because of the wide extent and wealth of subject material available and the space and time limitation imposed, presentation and discussion are less than originally planned. I—Losses and/or Values in Suspended Solids The weight involved in moving streams of industrial plant gases is commonly not appreciated, neither is their carrying power in the weight of solids maintained in suspension and moved with the gas stream from a point of origin or pick-up to a point of dissipation or settlement. These, however, are major weight figures; for example, in a modern iron blast furnace there may be five tons of gas for every ton of iron produced and by the time this blast furnace gas has been burned in stoves or under boilers the weight of gas discharged to atmosphere is on the order of eight times the weight of iron produced. Similarly for nonferrous metallurgy there may readily be from 10 to 20 times the weight of gases discharged to atmosphere as there is metal produced. A cement kiln in operation or a kiln in service to produce metallurgical lime may have on the order of 5 to 6 times the weight of stack gases as of clinker or lime produced, and at least the cement kiln, because of the very fine nature of its feed, is a very heavy dust producer. It may be noted that there have been two developments in progress for nearly three decades. Both are extraordinary in the industrial economics effected and in their ready availability to ever larger units of operation and their ever widening importance in industry, and both are productive of great quantities of finely divided material in furnacing. The first of these is the flotation process for ores, especially the metallics such as copper, lead, and zinc; and the second, powdered fuel combustion for power plant, industrial plants and metallurgical operations. Today, new developments, for example, flotation for the nonmetallics such as higher grade limestone for cement manufacture which requires still finer grinding and the powdered-coal-fired boilers with production ratings of over 1,000,000 lb of steam per hr, bring still more concentrated and hugely increased quantities of stack emission. Perhaps the honors for the greatest interest in the quantities and values escaping in waste furnace and equipment gases belong to the nonferrous metallurgical operations. Their record of achievement in the installation of dust and fume collection equipment, largely baghouses or Cottrell electrical precipitators, is exceeded by no other industry. Something of the magnitude and variety of equipment utilized in such recovery systems was covered by the writer in two papers presented to the Institute some 10 years ago.1,2 It is not intended to repeat the material of those articles, but it is thought that they complement this offering and should be noted. COPPER ROASTERS As the copper roasters are the first of the series of furnaces handling the copper-bearing concentrates in the usual copper smelter of today, it is in order to make them the first consideration. Multiple hearth sulphide roasters, not hard driven, often maintain their dust loss through exit gases at 3 pet or below of feed to furnace; in hard-driven or maximum-driven furnaces, exit gas losses often approximate 7 pet of charge with a ±2 pet variation for special conditions prevailing at some plants. A 5 pet loss of feed in a roaster gas exit, unless reclaimed, often makes the difference between a profit and loss operation, and in many cases substantial recovery is the very basis of dividend payments. As there is available very practical and successful equipment for the collection of the
Jan 1, 1950
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Institute of Metals Division - Steady-State Creep in Fe-2 to 11 At. Pct Si AlloysBy R. G. Davies
The activation energy for steady state creep above -500°C is observed to be independent of the applied stress although it varies from -67 kcal per mole at 2 at. pct Si to -100 kcal per mole at 11 at. pct Si due to changes in crystallographic order. The magnitude of the activation energy, by comparison with Fe-A1 alloys, indicates FeSi type of order in certain alloys. X-ray results confirmed the presence of FeSi type of order. It is proposed that dislocation climb is the rate controlling mechanism for all the alloys. It has been demonstrated that when a diffusion mechanism is the rate controlling process, the formation of a superlattice in brass,1 Fe3A1,2 Ni3Fe,3-5 and Feco6 1) increases the creep resistance, and 2) increases the activation energy for steady state creep. Furthermore, a study of creep in Fe-15 to 20 at. pct A1 alloys7 has revealed that as the alloy composition approaches the long-range order field, there is an increase in the activation energy for steady state creep which is thought to be due to an increase in short range order. Fe-A1 and Fe-Si alloys are similar in that they both form the DO3 superlattice in which aluminum or silicon atoms have only iron atoms as first and second nearest neighbors. There are, however, two important differences between the alloy systems: 1) The superlattice formation at -350°C commences at -10 at. pct si8 as compared to -20 at. pct Al,9 and 2) Fe-A1 alloys form a FeAl (B2 type) super-lattice where aluminum atoms have all iron first nearest neighbors even at 22 at. pct Al, but so far no similar FeSi superlattice has been observed. With the similarity between Fe-A1 and Fe-Si alloys in mind, alloys of iron with 2 to 11 at. pct Si were examined for variations with composition of the activation energy for steady state creep and of creep strength. The temperature range of greatest interest was above 1/2 TM (TM is the absolute melting temperature) where it is usually observed that diffusion is the rate controlling process. A subsidiary X-ray investigation of the Fe-Si system was undertaken in an attempt to define the position of the order-disorder boundary as a function of cooling rate. EXPERIMENTAL DETAILS a) Creep. Specimens whose gage length was 1.5 in. and with a cross-section 0.04 by 0.08 in. were strained in tension by a lever-arm arrangement, and the load was adjusted between each creep test to maintain constant stress. The apparatus and mode of operation have been fully described in a previous publication.7 As each test produced a creep strain of 0.25 pct, the variation in stress during the test was negligible. Creep strain was measured at the end of one of the alloy steel grips by a displacement transducer with the out-of-balance potential being recorded on a variable speed recorder. The full-scale deflection of the recorder could be varied in steps to give limits of sensitivity of between 0.1 and 0.001 pct creep strain. The alloys, Table I, were made available by the Metallurgical Department, National Physical Laboratory (N.P.L.), england,10 and by the Research Department, General Electric Co. (G.E.), Schenectady, N.Y. They were hot worked at -850°C, warm worked at 550° to 650°C, and recrystallized in vacuum at -750°C to give a grain diameter of -0.1 mm. All the alloys had a very low impurity content; those from the N.P.L., for which a complete analysis is available,'' show carbon less than 0.026 pct, manganese less than 0.006 pct, and oxygen plus nitrogen less than 0.0024 pct. b) X-ray Procedure. A General Electric XRD-5 X-ray set with a focussing lithium fluoride mono-chromator in the diffracted beam, and a pulse height analyzer to eliminate harmonic wavelengths of the cobalt radiation, was used to investigate the structure of several very fine grained (grain diameter <.01 mm) Fe-Si alloys after the following heat treatments: 1) Quenched from 700°C, 2) slow cooled from 650°C (-40°C per hr), and 3) very slowly cooled from 400° to 100°C (10°C per hr with a 24 hr anneal every 100°C). The method of obtaining the diffraction pattern over the range of 20 from 15 to 45 deg was to count for at least 100 sec every l/3 deg with a slit subtending 1 deg in 20 at the focus; the probable counting error was less than 2 pct.
Jan 1, 1963
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Part XI – November 1968 - Papers - Stress-Enhanced Growth of Ag3 Sb in Silver-Antimony CouplesBy L. C. Brown, S. K. Behera
The diffusion rate in Ag-Sb couples is sensitive to con~pressive load with the width of Ag3Sb, the only phase present in the diffusion zone, increasing with stress up to 800 psi and remaining constant above this. Kirkendall marker experiments show silver to diffuse much faster than antimony in Ag3Sb and incipient porosity may therefore develop at the Ag/Ag3Sb interfnce restricting the transfer of atoms from the silver into the diflusion zone. Application of compressive stress reduces the tendency for porosity to develop and so increases the growth rate. In a recent paper Brown et al.1 observed a significant increase in the thickness of Cu2Te in Cu-Te diffusion couples on application of a compressive stress as low as 20 psi. Similar stress effects have also been observed in the Fe-A1,2 Al-u,3 arid cu-sb4,5 systems. It has been suggested that the increase in growth rates of intermetallic phases in these systems is due to a decrease in the amount of Kirkendall porosity with applied stress. In the present paper, results are presented of the effect of compressive stress on diffusion in Ag-Sb, together with a detailed examination of the Kirkendall effect. The Ag-Sb phase diagram6 shows that antimony has a moderate degree of solid solubility in silver, 5.7 at. pct at 350°C, but that there is essentially no solubility of silver in antimony. There are two intermediate phases— (hcp7) from 8.8 to 15.7 at. pct Sb and Ag3Sb (orthorhombic8) from 21.8 to 25.9 at. pct Sb. EXPERIMENTAL Diffusion couples were prepared from fine silver of 99.95 pct purity and from antimony of 99.7 pct purity. Both the silver and antimony were produced in the form of discs 1/2 in. in diam by approximately $ in. thick, with surfaces ground flat to 3/0 emery paper. Diffusion anneals were carried out in the apparatus previously described.1 A compressive load was applied to the diffusion couple through a lever arm system, with a reproducibility estimated to be ±10 psi. All runs were carried out in a protective hydrogen atmosphere. Following the diffusion anneal specimens were sectioned and polished and the width of the diffusion zone was measured metallographically. Composition profiles were measured using an electrostatically focused electron probe with a spot size of 10 , counting on Sb L radiation. Corrections for matrix absorptiori and fluorescent enhancement9 were not required. S. K. BEHERA, formerly Graducate Student, Department of Metallurgy, University of British Columbia, is now Postdoctoral Fellow, Whiteshell Nuclear Laboratories, Atomic Energy of Canada Ltd., Pinawa, Manitoba. L. C. BROWN, Junior Member AIME, is Associate Professor, Department of Metallurgy, University of British Columbia, Vancouver, B.C., Canada. Manuscript submitted June 14, 1968. IMD RESULTS Fig. 1 shows an electron probe traverse of a typical diffusion zone. In all couples examined only one intermediate phase was observed and the composition of this phase, 23 wt pct Sb, was in good agreement with the composition of Ag3Sb, 23 to 28 wt pct Sb. The presence of this phase was confirmed by X-ray diffraction of filings taken from the diffusion zone. The probe traverses showed no detectable solid solubility in either the silver or the antimony although the phase diagram indicates that some antimony, up to 6.5 wt pct pct Sb, should be in solid solution in the silver. However the width of this portion of the diffusion zone would be expected to be very small in view of the low diffusion coefficient in the silver, 4 x 10-l6 sq cm per sec at 350°C, 10 compared with that in the Ag,Sb, estimated as 3 x 10-8 sq cm per sec in the present work, and this region would therefore not be expected to be seen in the probe traverse. Application of stress resulted in a significant increase in the width of the diffusion zone, Fig. 2. At 350°C, the thickness of Ag3Sb increased from 250 at 0 psi to 400 p at the limiting stress of 800 psi, indicating an apparent 150 pct increase in the diffusion coefficient. Similar behavior was also observed at 400°C, indicating that the stress effect is not characteristic of just one temperature. The growth of Ag3Sb at 350°C and at various stresses is shown in Fig. 3. In every case the growth rate was parabolic indicating diffusion control. The kinetic curves all passed through the origin showing that delayed nucleation of Ag3Sb was not responsible for the stress effect and that it was a real growth effect. A series of tests were carried out in which diffusion was allowed to take place at a lower stress following an initial high stress diffusion anneal. Speci-
Jan 1, 1969
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Extractive Metallurgy Division - Development of the Modern Zinc Retort in the United StatesBy H. R. Page, A. E. Jr Lee
From the inception of zinc retorting on a commercial scale in the United States in 1890,' the retort employed has undergone wide variations in its composition and manufacture, facilitating in part equally remarkable improvements in furnace capacities. The early day hand made clay retort was charged with carbonates or silicates or with coarse dead roasted concentrates mixed with a large proportion of charge fuel resulting in a relatively low zinc burden and fired 24 hr in direct coal fired furnaces. Its modern counterpart is fabricated in hydraulic presses from clay mixtures containing sizeable amounts of either silicon carbide or silica flour, charged with sintered flotation concentrates to more than three times the early day zinc burden and fired 24 to 48 hr in gas fired furnaces. This paper does not attempt to describe in detail the early day clay retort practice as it is well outlined in treatises by Ingalls,2 Lodin,3 Liehig,4 Hofman5 and others. A brief review of clay retort practice is presented together with a description of the major developments since 1912. Clay Retorts The Belgian type retort, both in the circular and elliptical forms, has been used almost exclusively. Typical dimensions of press made clay retorts around 1910 are shown in Table 1. Variations in these dimensions were used at different plants according to local conditions to a maximum inside diameter of 9 in. and inside length of 54 in. However, the effective heat penetration in a 24 hr firing cycle and the tendency of the retort to bend limited the retort size. Use of the elliptical vessel was an attempt to present a stronger cross-section resisting the tendency to bend and to increase the burden without increasing the depth of heat penetration. One exception to the 48-54 in. length was the 60 in. retort used as early as 1905 at Palmerton by means of supporting the last 12 in. at the butt end with a specially designed furnace back-wall. This backwall construction with the 60 in. retort had been developed and used at Bethlehem by G. G. Con-vers and A. B. DeSaulles. An attempt was made at Blende, Colo. to use even larger retorts of the Rhenish type based on European practice and requiring much higher furnace temperatures. Satisfactory plastic clays capable of withstanding these temperatures were not available, and the plant never operated successfully. PREPARATION OF BATCH Composition of the clay retort by weight was 40 to 50 pct raw clay and the balance "grog." Generally speaking the mix consisted of 7 parts plastic clay to 9 parts grog by volume. Principal source of the clay used was the Cheltenham vein—sometimes referred to as "St. Louis city clay." A typical analysis was A12O3-31.0 pct, SiO2-50.0 pct, Fe2O3-2.5 pct, MgO-0.3 pct, CaO-1.5 pct and loss on ignition 14.0 pct. At the smelter the clay was weathered whenever possible and then crushed to 0.08 in. or finer. Grog consisted of calcined adobies, cleaned retort scrap and cleaned refuse fire brick such as old furnace brick, blast furnace linings, and others. Saggers from ceramic plants and calcined flint clay were later used. The grog materials were ground to 0.12 m. or finer. Occasionally coke dust up to 10 pct of the mix was substituted for a part of the grog following European practice.² Particle size of the grog has a major influence on the retort properties—the larger the grain, the better can the retort withstand thermal shocks, resist bending at furnace temperatures and resist corrosion from slag; the smaller the grain, the lower the loss of zinc vapor through the retort walls. Grog forms the skeleton of the retort, and the clay shrinks around its grains to act as a binder. In the drying process, the grog has a stabilizing effect on the drying rate, decreasing shrinkage and giving up previously absorbed water to the surrounding clay to minimize the danger of cracking or checking.² Grog and clay were mixed through a horizontal pug mill with 10 to 20 pct water added, depending on whether the retort was to be formed by hand or mechanically, more water being required for the hand process. The batch or "mud" extruded from the pug mill was cut in convenient lengths for handling, stacked in piles or in special rooms, covered with wet burlap and allowed to "rot" or age from 1 to 8 weeks to increase plasticity. HAND MOLDING If the retort was to be molded by hand, the mud was repugged after the rotting period and given to the molders. Their molds consisted of 3 sheet iron or wood cylinders, each one third the retort length and defining the outer shape of the retort. Beginning with the bottom section, mud was placed in the form and tamped with a rammer
Jan 1, 1950
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Production - Domestic - Oil and Gas Development in Oklahoma in 1944By Raymond D. Sloan
During 1944, substantial gains were recorded in practically every phase of the petroleum industry in Oklahoma. With the spotlight of activity focused on other states during the more recent years, the production momentum that was achieved in Oklahoma through the discovery and development of such outstanding pools as Oklahoma City, Fitts. and major pools in the Seminole area during the late 1920's and early 1930's was practically spent by the end of 1943. However, with much of the industry's exploratory efforts greatly reduced in Illinois, Indiana and Kentucky, the strong demand for Mid-Continent crude and the optimism created by some discoveries in the state toward the end of 1943, Oklahoma has again become the recipient of much activity and interest, with its 1944 drilling activity, production and refinery runs to stills registering substantial gains over the preceding year. Development and Exploration Since the discovery of the West Edmond pool in April of 1943, with the substquent drilling and development boom, the scene of exploratory activity has shifted from the central. south and east portions of the state to the general trend of the . Granite Ridge, where leasillg and wild-catting were greatly activated within a wide radius of this high subsurface feature. Leasing activity, however, jumped the confines of the Granite Ridge trend and extended into all of the northwestern counties in the state. Seismograph activity at once began following and keeping pace with this shift in the leasing and exploration locale, by the concentration of a large number of seismograph crews in the area. At one time during the year,35 crews were concentrated in Oklahoma, the majority being west of the Granite Ridge and extending into the northwestern counties. To illustrate the increase in geophysical work done in the state during the year, records indicate that 377 crew months were worked in 1944, which is a 21 per cent increase over the 311.5 crew months activated in 1943. With the discovery in 1943 of several encouraging prospects and the finding of West Edmond as an incentive, drilling operations increased some 54.3 per cent, for a total of 1986 completions during the year. This is compared with a figure of 1287 for wells drilled in 1943, an increase of 699 wells. The industry, with a total of 1064 oil producers, enjoyed a success percentage of 53.6 per cent. Gas wells completed were 223, while 699 dry holes were drilled. In 1943, completions included 587 oil wells, 127 gas wells, and 573 dry holes. The number of oil producers completed during the Year was almost double the numher of wells in 1943. Of the total drilling wells completed in the state, 350, or 17.6 per cent, were wildcat operations—an increase of 5.1 per cent over the 194.3 total of 333. The wildcat success percentage was 13.4 per cent, 47 successful wells being completed for an average initial potential of 160 bbl. In the state, 23 gas wells were completed with an average initial production of
Jan 1, 1945
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Institute of Metals Division - The Third Stage of Work Hardening in Aluminum Crystals Deformed at 196°KBy A. Kelly, S. Sato
Tensile tests have been performed on aluminum single crystals of 99.99 pct purity at 196°K. The resolved shear stress when the stress-strain curve becomes concave to the strain axis depends on orientation, being always higher for crystals with an initial orientation close to the sides of the unit triangle. Observations have been made, with the optical microscope, of the appearance of slip lines on polished surfaces of the crystals. Particular attention has been paid to the first appearance of cross-slip. It is confirmed that marked cross-slip is first seen when the stress-strain curve becomes concave to the strain axis. Measurements are reported of the lengths of the slip lines observed on top and side faces of the crystals at various stages of the deformation. The lengths of the slip lines vary inversely as the flow stress for all crystals, independent of crystal orientation. From measurements of the lengths and separations of the slip traces it is possible to estimate the number of dislocations which are annihilated at each cross-slip site. It is concluded that the annihilation of screw dislocations of opposite sign is the most important cross-slip process occurring. FRIEDEL1 recently pointed out that the stress-strain curve of many pure metals of face-centered-cubic structure can be considered as composed of three stages. Plastic flow commences with a region showing a small rate of hardening which is approximately linear. This has been called "easy glide*. It is followed by a region of more rapid hardening in which the slope of the curve is again approximately constant and this, in turn, is superseded by a final part of the curve which is concave to the strain axis. Following Diehl2 we may designate these regions as stages I, II, and III respectively. The onset of stage 111 occurs at lower stresses at higher temperatures. The appearance of the slip lines formed during these various stages has been described by a number of workers?-5* The object of the present work was to make detailed observations of the lengths and separations of slip lines for a number of crystals of different orientations deformed at the same temperature and strain rate. Although much previous work has been published on the deformation of aluminum single crystals the importance of measurements of these quantities has only recently been realized—they are essential for experimental tests of recent theories of work hardening.' 9 In aluminum, deformed at room temperature, stage 11 of the stress-strain curve is very weakly marked, as the stress for the onset of stage 111 is attained soon after the end of easy glide. In the present experiments it was decided to use a temperature lower than room temperature so that stage II of the curve was better developed. However, at temperatures as low as 90°K slip lines are not measured easily with the optical microscope.5 For this reason 1960k was chosen as a suitable temperature. Even at 1960k however, stage III of the curve commences at glide strains of 6 to 10 pct and hence
Jan 1, 1960