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By R. P. Carreker

ONE of a series, this report is concerned with the experimental documentation of the deformation behavior of pure metals over a wide range of temperature. Previous reports in the series describe the creep behavior of platinum1 and aluminum2 and the tensile behavior of copper,&apos; silver,& and molybdenum.5 Subsequent reports will describe the creep behavior of copper and silver and the tensile behavior of platinum, thus providing extensive creep and tensile data on four face-centered-cubic metals tested under comparable conditions. Material Two lots of high-purity aluminum were used in this investigation. One lot, designated AC, was obtained direct from the Aluminum Co. of America as high-purity aluminum in notch-bar form. A typical analysis of this type of aluminum is 0.006 pct Si, 0.015 pct Cu, 0.006 pct Fe, and 99.975 pct Al. Lot BS was obtained from J. I. Hoffman of the Bureau of Standards as a portion of the Aluminum A described in his report of the redetermination of the atomic weight of aluminum.6 Lot BS originated with the Aluminum Co. of America also, and was received in the standard notch-bar form. A detailed chemical and spectroscopic analysis of lot BS has been published.6 Principa1 impurities were 0.006 pct Si, 0.003 pct Fe, 0.002 pct Cu, and >99.987 pct Al. Samples were processed identically by room-temperature swaging and drawing to 0.030 in. diam wires from approximately ½ in. diam rods that were machined from the notch-bar pigs. Samples were cut from the cold-drawn wire, placed in a grooved graphite block in groups of thirteen, and annealed in air for 1 hr at each of several temperatures, with the results shown in Table I. The two lots of aluminum responded quite differently to annealing, the behavior of aluminum AC suggesting that its grain growth was controlled by impurities. The recrystallization texture of aluminum of similar purity comparably treated has been reported as predominantly <111> fiber with some <100> fiber present.7 Testing Procedure The testing procedure and method of analyzing the data have been described previously.2,3 Annealed specimens of 5 in. gage length were tested in an Instron tensile testing machine at a constant head motion corresponding to a strain rate of 0.04 min-&apos; at a number of temperatures. Instantaneous tenfold rate changes were employed in some tests to deter-

Jan 1, 1958

By E. D. McMurry

INTRODUCTION Before discussing the use of the free piston; it may be well to explain briefly the type of gas lift valves with which the loo] is designed to function. The gas lift valve ii nothing more or less than a small back pressure regulator. It; construction consists of an outer hous ing covering a seamless metallic bellows in such a way as in form a sealed pressure vessel or pressure dome. To the bellow* in attached a stem and to this stem is attached a .rating member. When the valve is run into the hole, a pre-delermined pressure charge is placed in the pressure dome. As shown in Fig. 1. the valve is furnished in four different major assem-blies. to accomplish good results in different types of wells. The valve is mounted on a pup joint (Fig. 2a) : the eoin-plele assembly is entered into the tubing siring at the desired location. Each valve is furnished with a revere flow check valve (Fig. 2-b) to eliminate any back wash through the mechanism. Valve action is as follows: At any time the casing pressure is allowed to exceed the pressure forces within the pressure dome of the valve, the valve simply opens and passes gas from the rasing annulus into the tubing. When the casing pressure forces arc allowed to bleed to a force less than the pressure force within the dome, of the valve. the valve closes. With this type of construction. it is possible to open and close the valve or valves at will from the surface, the medium of the gas pressure in the rasing annnlus. The cycle of operation is governed by a tine cycle motor valve, commonly referred to as a gas lift interutitter or gas life surfacr controller (Fig. 3). In actual practice. after the well is unloaded only one valve is in operation . . . all other valve.: remain in the closed position. On pre-determined time cycles, it is possible to open and close this operating valve at will, and to pass the desired amount of gas through this valve wheneler needed. This method of gas lift is widelv used and has been found In be very efficient. However, it has long been known that even greater efficiency would be obtained if it were possible to place Piston between the injected gas and the fluid head. The free piston which will be discussed here was designed to accomplish this end and has been found to do so with very satisfactory results. DESIGN AND OPERATION OF THE FREE PISTON Basically. the free piston consist- of a telescoping assembly in which are incorporated the various control and operating parts (Fig. A set of sleeve valves which are opened and closed by movement of the telescoping section is contained in the. tool. A cross section of the free piston is shown in Fig. 4-11, &apos;rile main body cotain- a seamless monel bellows of the same type as that generally used in pressure charged gas lift valves (Fig. 4-c), and a valve core to permit placing a pressure charge in the bellows before the free piston is placed in service. The bellows is the main control unit of the free piston and performs two function: 1. It governs the opening and closing of the sleeve valves. a.: dictated by the producing activities of the well in which the piston is operating. 2. In its normal position, it holds a rubber packer in an elongated position to permit passage of fluid between the packer and the tubing walls. The lower section of the free piston contains a hydraulic shock absorber which cushions the return of the tool to its

Jan 1, 1953

By J. Lindbo, B. Vigeholm

IN transmission electron microscopy, specimen thicknesses quoted are frequently based upon either traditionally familiar values or a few evaluations representing the whole material. Taking aluminum in 100 kv TEM as an example, average and maximum values are widely accepted as being 2000 to 2500 and 6000 to 7OOOÅ, respectively. It is the purpose of this note to revise these figures and to point out the importance of evaluating individual specimens carefully. All evaluations have been based upon slip trace widths and lattice orientations as determined from diffraction patterns. In many cases where two or more slip systems have been operating the geometrical method described by Crocker and Bevis1 has been applied as a check. The foils were usually oriented to within 2 deg from the exact Bragg angle. Kikuchi patterns were used as indications of correct orientations but not applied in the evaluations. The tilt of the foil surface relative to the beam normal may with certain geometrical relations between the tilt axis and the operating slip plane lead to substantial errors.2&apos;3 Where these geometries were inevitable the samples were omitted in the investigations. Various measures were taken in order to overcome ambiguities, e.g., comparison with neighboring grains, tilts, evaluations based upon two or three slip systems,&apos; and comparison with extinction contour evaluations where s = 0 conditions were obtained. Errors caused by misinterpretation of the slip traces on a micrograph are easily avoided by considering the bright-dark sequence on opposite surfaces and by taking into account the tapering of the foil usually leading to a distinguishable divergence of the pair of traces. In the investigations described here the interpretation was further facilitated as the slip trace formation was observed on the microscope screen and sketches taken down. In a few observations slipping was so violent that the distinction of pairs was considered dubious and consequently given up. To assess average values, thickness evaluations carried out in two independent investigations were analyzed: I) 99.998 pct A1 extruded, cold-drawn, and recrys-tallized to grain sizes between 35 and 500 um were deformed in tension at room temperature. In order to determine the dislocation densities as a function of strain,4 specimens prepared by spark machining and electropolishing in a PTFE holder were analyzed in the electron microscope at 100 kv. Thicknesses were evaluated for 569 selected areas. Histogram I in Fig. 1 shows the results, the average thickness being 4900Å. II) Electropolished specimens prepared from 99.9999 pct A1 with magnesium contents from 0.005 to 0.5 pct rolled to foil and annealed were subjected to fission fragment irradiationa2 For volumetric dose and defect concentration determinations thickness evaluations were performed on 123 areas. Histogram II in Fig. 1 shows the thicknesses of these areas averaging 4250Å. Whereas in investigation I no selection related to thickness has been made, some thin as well as thick areas have been omitted from I1 for experimental reasons. This and the application of two different microscopes although of the same type may account for the difference in average thickness. Assuming a mean error of 10 pct for a single evaluation, the error of the average should be negligible. In order to investigate the maximum transmissible foil thickness in aluminum, specimens were prepared from single crystals with (111) and (110) orientations parallel to the beam, and from polycrystalline material. Maximum values of thickness that could be measured were given by the stopping of the dislocations. The visibility often extended far beyond the end of the slip trace, but with no means of knowing the

Jan 1, 1970

By E. J. Ripling, S. I. Liu

IT has been shown in a number of recent publications that much information on the mechanical behavior of metals can be gleaned by first deforming test specimens under one set of conditions, and then evaluating the effect of this deformation by means of a subsequent tensile test. A straining procedure of this type has been applied to study the flow behaviors of a number of metals.1, 2 In these studies the prestraining and testing were both tensile strains, while the straining temperature was varied between the prestraining and testing steps. These data indicate that there is a more or less general flow behavior exhibited by all metals which are pre-stretched at one temperature and then tested in tension at a second temperature. Prestraining a metal at a high temperature produces a lower yield strength during the subsequent low temperature strain than would the same total strain at the lower temperature. On reversing the order of the strains, low temperature prestraining produces a higher yield strength during the subsequent high temperature straining than would a single high temperature strain of the same magnitude. Unlike the flow behaviors, the fracturing characteristics of metals when prestrained under one set of conditions and tested under a second set of conditions is quite material dependent. The fracture behavior of a number of steels2" as well as of a commercially pure zinc,4 have been investigated by these two-step tests and was found to depend upon the position of the transition temperature with respect to the prestraining and testing conditions. Since these fracturing phenomena are complicated by the appearance of the transition temperature, it has been difficult to reliably define the basic effect of a two-step straining procedure in fracturing. Metals crystallizing in the face-centered cubic system do not exhibit transition temperature effects so that the mechanical characteristics obtained on these materials could serve as a base for two-step straining behaviors. Consequently groups of specimens of the aluminum alloy 24s-T4 were prestrained various amounts at room temperature in either tension or compression after which these strained specimens were further strained to failure, or tested in tension, at either room or some lower temperature. Other groups of 24S-T4 specimens were prestretched at various low temperatures after which these were tested in tension at room temperature. These straining techniques then made it possible to compare the behaviors of aluminum with the behaviors previously presented for steels. Material and Procedure The commercial aluminum alloy 24S-T4 in the form of 3/4 in. rods was used in this investigation. The material was subjected to the following treatments before machining: 1—resolution treating at 920" & 10°F for 45 min, 2—quenching in water at room temperature, and 3—aging at room temperature for four days. The re-heat treated material was then machined to either of the specimen shapes shown in Fig. 1. Fig. la shows the threaded-end specimen used for prestraining in compression. Fig. 1b shows the specimen used for both prestrain in tension and final testing. The material subjected to precompression in the form of the specimen shown in Fig. la was re-machined to the specimen shape in Fig. 1b for final testing. Prestraining in tension and final testing were done without any intermediate machining. All straining was performed on a 10,000 1b Riehle tensile testing machine. Tensile strains were conducted in a specially designed concentric fixture which produced an eccentricity of less than 0.001 in." The change in diameter at the minimum section of

Jan 1, 1954

By Garth M. Crosby

Hugh E. McKinstry (Professor of Geology, Laboratory of Mining Geology, Harvard University, Cambridge, Mass.) Pre-Cambrian age for the Coeur d&apos;Alene mineralization, as indicated by isotope studies and recently discussed by Silverman, Long, and Kulp&apos; would explain some features of the mineralogy of the district that have long been a puzzle. In the Silver Belt, especially in the Sunshine mine, lead-zinc min erali zation passes downward into tetrahedrite ore. Although commercially speaking this is a rich silver zone, the silver is, quantitatively, a mere impurity amounting to a small fraction of 1 pct. In effect the zonal change is from lead-zinc down into copper mineralization—-the usual zonal change that occurs in many districts. In the Burke-Mullan portion of the district, on the other hand, lead-zinc ore does not pass downward into copper mineralization of the Sunshine type. Instead, pyrrhotite appears in depth while the tenor in lead and zinc declines. The change occurs at increasingly greater depth away from the Gem stocks, deepening irregularly by some 3000 ft within two to four miles. As noted by Crosby, biotite, grunerite, and garnet appear in the deep zone. The marked difference between this apparent zonal change and the more nomal change to a copper zone is quite explainable if already existing pre-Cambrian veins have been locally metamorphosed by a Tertiary intrusive. The chief obstacle to this explanation is the evidence that mineralization cuts Laramide intrusives, but evidence on this point is conflicting as indicated by Crosby&apos;s observations and summary. This is not the first instance of a problem in determining the time-relationship of mineralization to a spatially associated intrusive. At the Noranda mine veins of chalcopyrite extend into a diabase dike which apparently cuts the ore, although Price2 concludes that the ore is later. However, at the Normetal mine diabase of a similar dike is thought3 to intrude the orebody but is cut by stringers of chalcopyrite. In the Sullivan Mine, B. C.,4 galena follows a fracture in a larnprophyre dike which, itself, cuts the main orebody. In the Sudbury district dikes of olivine diabase are clearly younger than the nickel ore, yet where they cut the Creighton orebody they contain stringers of chalcopyrite. In the laboratory, Hawley5 has developed veinlets of sulfide (chalcopyrite) it] silicate gangue by heating specimens of ore in a stream of H2S at 410 °C. From this and other evidernce. it seems clear that sulfides can be transferred from one site to another — at least through short distances — at temperatures well below their melting points. It would seem then that even if sulfide Mineralization in the Gem stocks can be shown unequ ivocably to be later than the intrusive the possibility of "remobiliza tion" need not be more than local. Thus the zonal relationships are quite in accord with a pre-Cambrian age for original deposition of the lead, zinc, copper, silver, and uranium in the Coeur d&apos;Alene district. REFERENCES 1. A. Silverman, A. Long, and J. L. Kulp: Discussion of: The Gem Stocks and Adjacent Orebodies, Coeur d&apos;Alene District, Idaho. Mining Engineering, May 1960, pp. 470-471; AME Trans., 1960, vol. 217, p. 117. 2. Peter Price: Geol. & O. D. at the Home Mine, Noranda, Quebec. Can. Inst. M & M Bull 263, 1934, p. 108; also,Trans. CIMM 1939, pp. 108-140. 3. w. L. Brown Nometal Mine in structural Geology of Canadian Ore Deposits, Montreal, 1948, p. 690. 4. C. O. Swanson and H. C. Gunning: Geology of the Sullivan Mine. Can. Inst. Mining & Met. Trans. vol. 48, 1945, p. 653. 5. J. E. Hawley: Heat Effects on Sulphides and Possible Applications. Univ. Toronto Studies, Geol. Ser. No. 46, 1941, p. 34.

Jan 1, 1961

By H. C. Vacher, C. J. Newton

EXTENSIVE investigations in the field of residual strain measurement by X-ray diffraction have been made by Bollenrath, Hauk, and Osswald,1 by Smith and Wood,2&apos;3 by Greenough; by Rosenthal and Norton." and many others. Since X-ray strain measuremeits apply only to those crystals of the test body which are of the proper condition and orientation to diffract and since the residual strains revealed may be accompanied by either body or tex-tural stresses, there has been considerable disagreement among investigators with respect to the validity of conclusions in this field. Although the experi-mentors have employed a variety of loading schemes, surface preparations, and X-ray wave lengths, the observations almost invariably have been made only on the outer surfaces of the specimens. The present note is not to be construed as an exposition of a new method of stress analysis by X-ray strain measurements on sections but as a presentation of some results which point to interesting possibilities for further experiments with sections. The two test rods used in this study were of ingot iron annealed at 910°C. The initial length of the gage section was 2 in. and the diameter was 0.415 in. Cross-sections were cut from the ends of the annealed rods to provide strain-free material. The tensile rod was axially loaded the desired amount in a commercial testing machine. A 1 in. portion of the gage length was cut from the other rod and was subjected to compression in the same machine. Details of this plastic straining of each rod are given in the upper half of Table I. A half-cylinder piece about 1/4 in. long was obtained by making a short longitudinal plane cut containing the axis of the rod near the center of the gage length. From adjacent material a disk about 1/8 in. thick was cut to provide the cross-section specimen. Later another section was cut from this same region with an angle of 30" between the normal to its surface and the axis of the test rod. A cross-section and a longitudinal section were cut from the compression rod in a similar manner. All of these as well as the strain-free cross-sections were mounted in Bakelite and used as specimens for the following X-ray strain measurements. During the course of the study, it became apparent that the condition of the surface of a specimen was a highly critical factor. One of the annealed strain-free specimens as a control was subjected to about 24 hr of polishing with fine alumina, interrupted about every 2 hr for etching with 1 pct nital. Its lattice parameter was determined at intervals from measurements on back-reflection X-ray diffraction patterns, which were calibrated with diffraction from tungsten powder. The parameter gradually approached the value found in the literature for strain-free iron and remained there, within the limits of the experimental error. This determined a long polishing and etching procedure which was adopted for all the specimens and which gave X-ray results from the surfaces believed to be representative of each specimen as a whole. A large number of back-reflection patterns were made with cobalt and chromium radiation, all at normal incidence. Except for some preliminary stationary exposures made to monitor the removal of cold work from the surfaces, each exposure was made with the specimen slowly translating and the film slowly rotating. In appropriate cases a thin layer of a standard metal powder, tungsten with cobalt radiation and silver with chromium, was dusted over a film of vaseline on the surface of the specimen to serve to calibrate the X-ray patterns. After the preliminary work, four films were made,

Jan 1, 1956

By J. P. G. Farr, R. Brownsword

THE role of solute segregation in the formation of cellular solidification substructures in tin and its dilute alloys is well-established, see, e.g., Ref. 1. Segregation has been shown to persist during cooling, enabling solidification structures to be studied from sections taken at some distance behind the interface. In the present work, a single crystal of commercial nickel, 99.965 pct, was examined in this way. The crystal was cut from the center of a rod given a single pass in an electron beam floating zone melter. Polished sections of a nickel specimen taken normal to the growth direction showed a very fine precipitate phase, the distribution of which varied over the section. The identification of the phase proved difficult because of the small amount present and the small particle size, about 1 p: but it was shown by probe microanalysis to contain only nickel and oxygen in detectable concentrations and was probably nickel oxide, NiO. Bulk analysis of the material before melting showed there to be only 3 to 4 ppm of oxygen present, thus demonstrating a very considerable segregation concentration effect. In some areas of the section the precipitate formed a discontinuous hexagonal network suggesting decoration of the cellular boundaries known to be present in the sample2 whereas in a restricted region the precipitate formed small clusters. Occasionally it could be seen that the clusters were at the intersections of an hexagonal network of cellular dimension. It was suggested3 that this was the result of enhanced segregation to the cell boundary intersections whereas general cell boundary segregation was insufficient to give a precipitate. Enhanced nodal segregation has since been demonstrated in a number of systems.1, 4-8 The development of a suitable electrolytic etching technique (perchloric acid 20 pct v/v; ethyl alcohol 70 pct; glycerol 10 pct; current below electropolishing plateau; 1 to 2 sec etching) suggested the association of the phase with regions of solute segregation (where ko < 1); in these regions anodic attack produced grooves or depressions. In a study of the variation of solidification substructures with degree of constitutional supercooling, Biloni et a1.&apos; appear to have used standard growth conditions and varied the solute concentration. They were able to produce in a series of individual tin crystals examples of substructure ranging from planar interface through various cellular structures to den- Fig. 1—Electroetched section taken normal to the rod axis; the center of the rod lies to the left and the periphery to the right of the micrograph. The variation of structure across the section is evident. Magnification 60 times. drites. It was possible in the present nickel crystal to observe a continuous range of substructures varying with degree of supercooling across a single section as shown in Fig. 1. Growth rate, 13 mm per min, and temperature gradient were essentially constant; the variation in structure is thought to be due to a radial gradient in solute concentration ahead of the solid interface. The liquid at the interface is likely to have been richer in solute toward the periphery of the zone, the result of curvature of this interface. The type of substructure was seen to vary with increasing constitutional supercooling as follows: a) region free of precipitate. top left, Fig. 1: 6) region of nodal precipitates which became arranged in hexagons on passing from the center of the rod: c) irregular hexagonal cells with incomplete boundary precipitation; d) regular hexagonal cells of decreasing size with complete boundary precipitation. Fig. 2 shows the transition from stage 6 and Fig. 3 shows the structure in stage d. Within stage 0, the range of conditions over which irregularly positioned nodes occur appears to be small and the nodes are soon recognizable as taking up positions at the intersections of an hexagonal network as the supercooling increases.

Jan 1, 1970

By Dwight H. Seely, Louis R. Records

A process for low-temperature dehydration of natural gas utilizing Joule-Thomson effect in expansion through a throttling orifice has been tested in a full-scale field installation. The results of these tests are presented in the form of performance curves from which the process may be easily evaluated. The effect of separation temperature on condensate recovery from the process is also shown. INTRODUCTION The transportation of natural gas from producing well to the consumer has always encountered the problem of hydrate prevention. This problem has become increasingly important in the past ten years due to the rapid increase in produced gas volumes, production pressures, transportation pressures and distance from producing wells to consumer. Natural gas, as normally produced from gas or gas-condensate wells, is saturated with water vapor at well-head conditions of temuerature and pressure. The solution of the hydrate problem require; but one basic process — dehydration of the gas to a water content which will result in a water dew-point below the minimum temperature to be encountered from the producing well to the point of consumption. Much of the recent development of gas and gas-condensate reserves in the Gulf Coast Area has been in locations which are accessible only by water. High well-head pressures, pipeline construction and maintenance costs and the desirability of final central gas-condensate separation facilities have stimulated the development of dehydration equipment which can be installed at each well and which will permit hydrate-free transportation of both gas and condensate in the same line to central facilities. There are four types of natural gas dehydration processes now used: 1. Adsorptive processes. 2. Absorptive processes. 3. Chemical reaction processes. 4. Refrigeration processes. The first three of these processes are indirect in that they require use of adsorbents, absorbents or reactive chemicals. These materials require regeneration and part of the total gas stream is consumed in the regenerative process. Indirect processes have a wide range of flexibility as defined by allowable operating pressure and temperature, but most are not easily adapted to automatic operation. The refrigeration process described in this paper was designed for installation at the producing well-head. It requires no regenerative cycle and with normal well-head temperatures no external source of heat. The flexibility of this process is limited only by the pressure drop which may be allowed between well-head and transportation line. THEORY There are three basic physical concepts involved in the low temperature dehydration process. These are: 1. Formation of hydrocarbon hydrates. 2. Joule-Thompson effect resulting from the expansion of gaseous mixtures through a throttling orifice. 3. The equilibrium composition characteristics of water vapor and gaseous hydrocarbon mixture.. The chemical composition and physical structure of hydrate; have been described by several investigators.3,4,5,10 Specific conditions of temperature, pressure and composition as well as the requirements for turbulence and presence of free water necessary for hydrate formation have been described by Katz.6 Natural gas hydrates, as they are found in plugged gas pipe lines, have the appearance of packed snow. The mass of these hydrates has low continuous porosity and permeability. Joule-Thomson effect. or the reduction in temperature which occurs when natural gas is throttled throusll a restrictive orifice, is the basic phenomenon which permits efficient use of refrigeration for the purpose of dehydrating natural gas. Joule-Thomson coefficients for gafeous mixture; of methane with ethane and with butane have been reported by Buder.-I~olzer, Sage and Lacey.2 Brown1 predicted temperature drops for pressure drops from enthalpy-entropy calculations. Aside from this work there were no fundamental data found which would be applicable to natural gas mixtures of varying spe-

Jan 1, 1951

By Dwight H. Seely, Louis R. Records

A process for low-temperature dehydration of natural gas utilizing Joule-Thomson effect in expansion through a throttling orifice has been tested in a full-scale field installation. The results of these tests are presented in the form of performance curves from which the process may be easily evaluated. The effect of separation temperature on condensate recovery from the process is also shown. INTRODUCTION The transportation of natural gas from producing well to the consumer has always encountered the problem of hydrate prevention. This problem has become increasingly important in the past ten years due to the rapid increase in produced gas volumes, production pressures, transportation pressures and distance from producing wells to consumer. Natural gas, as normally produced from gas or gas-condensate wells, is saturated with water vapor at well-head conditions of temuerature and pressure. The solution of the hydrate problem require; but one basic process — dehydration of the gas to a water content which will result in a water dew-point below the minimum temperature to be encountered from the producing well to the point of consumption. Much of the recent development of gas and gas-condensate reserves in the Gulf Coast Area has been in locations which are accessible only by water. High well-head pressures, pipeline construction and maintenance costs and the desirability of final central gas-condensate separation facilities have stimulated the development of dehydration equipment which can be installed at each well and which will permit hydrate-free transportation of both gas and condensate in the same line to central facilities. There are four types of natural gas dehydration processes now used: 1. Adsorptive processes. 2. Absorptive processes. 3. Chemical reaction processes. 4. Refrigeration processes. The first three of these processes are indirect in that they require use of adsorbents, absorbents or reactive chemicals. These materials require regeneration and part of the total gas stream is consumed in the regenerative process. Indirect processes have a wide range of flexibility as defined by allowable operating pressure and temperature, but most are not easily adapted to automatic operation. The refrigeration process described in this paper was designed for installation at the producing well-head. It requires no regenerative cycle and with normal well-head temperatures no external source of heat. The flexibility of this process is limited only by the pressure drop which may be allowed between well-head and transportation line. THEORY There are three basic physical concepts involved in the low temperature dehydration process. These are: 1. Formation of hydrocarbon hydrates. 2. Joule-Thompson effect resulting from the expansion of gaseous mixtures through a throttling orifice. 3. The equilibrium composition characteristics of water vapor and gaseous hydrocarbon mixture.. The chemical composition and physical structure of hydrate; have been described by several investigators.3,4,5,10 Specific conditions of temperature, pressure and composition as well as the requirements for turbulence and presence of free water necessary for hydrate formation have been described by Katz.6 Natural gas hydrates, as they are found in plugged gas pipe lines, have the appearance of packed snow. The mass of these hydrates has low continuous porosity and permeability. Joule-Thomson effect. or the reduction in temperature which occurs when natural gas is throttled throusll a restrictive orifice, is the basic phenomenon which permits efficient use of refrigeration for the purpose of dehydrating natural gas. Joule-Thomson coefficients for gafeous mixture; of methane with ethane and with butane have been reported by Buder.-I~olzer, Sage and Lacey.2 Brown1 predicted temperature drops for pressure drops from enthalpy-entropy calculations. Aside from this work there were no fundamental data found which would be applicable to natural gas mixtures of varying spe-

Jan 1, 1951

By P. T. Bail, J. E. Bobek

In reservoirs containing soft shales interbedded with oil-producing sands, it is possible to have water movement from the shales into the sands during reservoir depletion. This paper presents the results of scaled flow-model tests performed to investigate the efficiency of oil displacement by this vertical influx of water into oil-producing sands. In these model tests, the effects of rate of influx and rock wettability were considered. Oil recoveries by shale-wafer influx and by water flooding were cornpared after 0.4 hydrocarbon volume of water entered the producing sand. This comparison was made for water-wet and oil-wet systems. In water-wet sand, shale-water influx produces slightly less oil than conventional water flooding; in oil-wet sand, shale-water influx produces about one-half as much oil as conventional water flooding. In another type of comparison, it was found that shale-water influx followed by water flooding recovers less oil than water flooding alone. This is true for both water-wet and oil-wet sands. A comparison of tests run at different rates of shale-water influx shows that oil recovery is insensitive to rate in water-wet sand; in oil-wet sand, oil recovery decreases with decreasing rate of influx. INTRODUCTION Localized subsidence of the earth&apos;s surface has accompanied the depletion of some oil reservoirs, particularly in California,1, 2 along the Texas Gulf Coast,3 4 and in the Bolivar Coastal fields of Venezuela. Subsidence occurs when fluid withdrawals reduce the pressure in the reservoir. The reasons for subsidence accompanying a reduction in reservoir pressure are not known with certainty.10° However, there is considerable evidence that compaction of soft shale beds adjacent to producing oil sands can be a major cause of this subsi-dence.3, 6, 10-12 When the shales compact, a limited amount of water moves from the shales into the producing sands. A schematic illustration of this oil-producing mechanism is shown in Fig. 1. As the pressure in the sand declines due to oil production, a predominantly vertical pressure gradient develops at the sand-shale boundary. This causes water to move from the shale into the sand as indicated by the solid arrows. This paper reports the results of scaled flow-model tests to investigate the efficiency of oil displacement by the vertical influx of shale water into producing sands. The model tests were not performed with the aim of duplicating the recovery behavior of any specific reservoir. The primary purpose of the tests was to obtain a better understanding of oil displacement by shale-water influx. A knowledge of the oil- and water-production characteristics of even a simplified reservoir system should be of value to engineers estimating the performance of reservoirs where shale-water influx is occurring in conjunction with other production mechanisms. The following limitations and assumptions apply to the model work. 1. The sand of the prototype reservoir is homogeneous and horizontal. 2. The shale-water influx is uniformly distributed along the top and bottom of the sand member being studied. 3. No effects of edge-water drive or dissolved-gas drive that might accompany shale-water influx are considered. PROTOTYPE RESERVOIRS Scaled-model tests were performed to study oil displacement from three prototype reservoir sections. The reservoir sections modeled consist of single sand layers out of a sequence of -sand and -shale layers, as illustrated in Fig. 1. Each prototype represents a homogeneous, high-permeability, unconsolidated sand layer. In the field, the prototype is oriented in such a manner that one end is at the radius of drainage of a producing well and the other end is pointed toward the producing well (Fig. 2). The sand and fluid properties and the dimensions of the three prototypes are given in Table 1. The capillary pressure relationships for the three prototypes are presented in Figs. 3, 4 and 5. The oil-water per-

By L. H. Robinson

Triaxial compression tests on Indiana limestone indicate that chemical additives in the pore fluids can increase or decrease the strength in plastic failure but not in brittle failure. Tests using a series of the sodium salts of dicarboxylic acids show that odd-number carbon-atom chains decrease the yield strength as much as 3.0 x 10 3 psi, and even-number carbon-atom chains increase the yield strength as much as 9.0 x 102 psi. ,The most effective chemical (sodium citrate) decreased the yield strength of Indiana limestone from 16.0 x 103 to 12.0 x 103 psi. The chemical additives investigated have no influence on microbit drilling rate when drilling with zero differential pressure. However, when drilling at a 2.0 x 103-psi pressure differeniial and using an odd-number carbon chain compound as the circulating fluid, the roller bit drilling rates were slower than with water whereas the drag bit drilling rates were faster. One even-number carbon chain compound added to the circulating fluid produces the opposite effect: the roller bit drilling rate is slightly faster than with water and the drag bit slower than with water. INTRODUCTION A Russian book by Rehbinderl published in 1944 generated much interest in the possibility of aiding and accelerating the destruction of solids by the action of a liquid in which the solids are deformed. This book describes a process in which microcracks are generated during elastic deformation. To describe this process, the rock is divided into three zones: (1) the zone in which the destruction takes place, (2) the predestruc-tion zone (an affected area immediately below the destroyed zone) and (3) the undisturbed specimen. Consider a load applied normally to a surface of an infinite slab of rock. Immediately below the point of application of the load, the rock is destroyed by compression or shear forces. Below this area of destruction, because of a great number of discontinuities ranging from defects to weak points in crystals of discontinuities in crystal latices, very small cracks are created in or between the crystals (often referred to as microcracks). Upon removing the load, the broken rock in the destroyed zone could be removed. In the lower predestruction zone, however, the microcracks in and between the crystals could disappear by the process of rehealing, i.e., the molecular attraction from one side of the crack to the other side being sufficient to completely eliminate the crack. Thus, a large number of these microcracks possibly exist only for a relatively short period of time. The concept of small cracks being generated within the crystals of a rock is not unreasonable. If the rock matrix is deformed below the yield point, some of the defects present within the crystalline structure could start small cracks through the interior of the grains. Upon removal of the load, these microcracks reheal (or the newly generated surfaces come back together) so that all evidence of cracks completely disappears. Under various types of loading, and in various types of fluids, the rehealing of these cracks would be time dependent. If a liquid adhered to the surface of a rock, it could penetrate into the microcracks and thus delay or prevent the rehealing process. This suggests that the prevention of healing of the microcracks may be dependent upon the wetting characteristics of the solid. Thus, rocks which are water-wet should be more easily destroyed in water than in nonpolar hydrocarbon liquid. Adsorption of a liquid could also reduce the free surface energy which could explain the decrease in strengths of materials under nonrepetitive-type loading. Rehbinder&apos;s work prompted Boozer, Hiller and Serdengecti 2 to examine the effects of pore fluids on the deformation of rocks subjected to triaxial compression over a range of confining pressures, temperatures and strain rates. Fluids which strongly adsorbed on the rock grain surfaces decreased the strength of sandstone and limestone, which deformed plastically. For certain strain

By E. E. Barker

ALTHOUGH flotation was known to be a successful process prior to 1912, Utah Copper Co.&apos;s ores were not entirely treated by this process until 1923. Experiments had been conducted, of course, prior to that time, and in February, 1917, the first unit of the Arthur plant was changed over from gravity concentration to flotation. On May 16, 1918, the entire Arthur plant was on flotation, excepting the coarse concentrate which was tabled prior to fine grinding. The reasons for the delay in adopting flotation at these plants were, first, that it was decided to await the outcome of the litigation with the Butte & Superior Mining Co., which began with an injunction served on Oct. 3, 1911. This litigation continued for years. Then the demands on the plants in the war years 1916, 1917 and 1918, really precluded any further drastic changes during that period, as all efforts were bent on maximum tonnage, and the cry of tonnage, rather than of recovery, was the major issue. The postwar depression followed these years of intensive production, so that it was not until 1922 that the Magna plant was equipped to use this process. Excepting, then, the amount of coarse concentrate that was tabled, 1923 was the first year when the Utah Copper Co.&apos;s ores were on, a full flotation basis. EFFECT OF FLOTATION ON ORE RESERVES The object of this paper is to point out the effect that flotation has had on the operations of the Utah Copper Co. In 1905, when D. C. Sackling began making history in copper, the ore reserves were 34,000,000 tons, with a grade of 2 per cent. copper and a mill capacity of 700 tons daily. The point of cut-off between nonprofitable and profitable grades was 1.2 per cent. A few years later the capacity was increased to 6000 tons, when 1.1 per cent became the point of cut-off. Ore reserves had climbed to 80,000,000 tons, having a grade of 1.9 per cent. In 1911 there was an ore reserve of 300,000,000 tons, with a grade of 1.5 per cent and a cut-off of 1 per cent.; in 1918 the ore reserve was approximately 400,000,000 tons, and a grade of 1.38 per cent., and point of cut-off 0.95 per cent., based on normal costs and prices. Up to this

Jan 1, 1928

Discussion of the paper of HOWLAND BANCROFT, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 91, July, 1914, pp. 1767 to 1769. THEODORE SIMONS, Butte, Mont. (communication to the Secretary*). -While preparing maps and models for use in mining litigations the writer was frequently confronted with the problem referred to in Mr. Bancroft&apos;s paper. His chart gives the apparent angle of dip with which a vein should be plotted on a vertical section not at right angles to the strike of the vein. For a quick determination of this apparent angle the writer has used an exceedingly simple graphical method, which he believes may prove helpful to engineers engaged in practical work. It is submitted, not as a criticism of Mr. Bancroft&apos;s paper, but as a means of solving the same problem when no chart is available and when calculations would consume too much time. The writer&apos;s method requires merely a few lines marked off on a piece of tracing cloth, as shown in Fig. 1: Draw line be on any convenient scale. At b erect a perpendicular, ba. By means of a protractor cut off on ba a number of angles within the probable range of variation of dip, so that a line connecting a and c, for instance, forms an angle of 60° with be, etc. With b as a center and be as a radius, draw a circle through c. This completes the tool for solving the problem. Fig. 2 represents the line of strike of the vein and db the trace of the vertical plane on which the vein is to be plotted with the apparent angle of dip. A° is the angle which this plane makes with the strike. Fig. 3 shows the application of the method: Place line cb of tracing over line db of Fig. 2 and move fore and back until line of strike becomes tangent to the circle. Connect d with the point (a) that marks the true angle of dip as found by measurement in the mine (60° in the case illustrated). The angle adb is the apparent angle of dip (C°) to be used in the vertical section. Proof.-As stated in Mr. Bancroft&apos;s paper, the apparent angle of dip is: tan C° = sin A° tan B° (1)

Jan 12, 1914

By P. D. Hunt, B. Tani, M. G. Chasanov, R. Schablaske

The Zn-Vphase diagram was studied by thermal. metallographic, X-ray, and sampling techniques. Three ternary phase equilibria were observed: Mutual solid solubilities in vanadium and zinc appear to be negligible. The liquidus line is retrograde from 670° to 756°C. 1 HE only information in the literature relating to the Zn-V system was a study of corrosion of vanadium by liquid zinc&apos; and an examination of the effectiveness of zinc coatings in protecting vanadium-base alloys from oxidation at high temperatures.2 Establishment of the Zn-V phase diagram was undertaken as part of a study of transition metal solubilities in liquid metal solvents. Chemical, metallographic, thermal, and X-ray diffraction analyses were used to determine the diagram. MATERIALS AND EXPERIMENTAL PROCEDURES Vanadium (99.86 pct) in the form of powder and small chips was employed. Stick zinc (99.99 pct; major impurities: 10 to 15 ppm Pb and 20 ppm Cu) was used in the liquidus determinations and thermal analyses; zinc powder (98.80 pct) was used to prepare intermediate compositions. The liquidus lines were determined by chemical analysis of filtered samples of the saturated melts. The apparatus and sampling techniques were similar to those described by Martin, et al.3 The entire metal sample was dissolved to preclude analytical errors due to segregation on cooling. Vanadium was determined amperometrically, using iron (11) as the titrant,4 to an estimated accuracy of 1 pct. Standard techniques of thermal analysis were employed to examine alloy specimens contained in alumina crucibles under helium. Heating and cooling rates were about 1°C per min. At least five heating and cooling cycles over the range 420° to 700°C were performed for each of two Zn-15 pct V alloys. A Zn-0.2 pct V alloy was used in the determination of the eutectic temperature. The separation of intermediate phases from zinc-rich alloys was carried out by selective leaching with ammonium nitrate solutions. For further investigation of intermediate phases 1/4 in. diam powder compacts were prepared by pressing at 80,000 psi and were annealed in argon at 415" to 450°C for 10 days. Larger quantities of intermediate phases were prepared in sealed tantalum capsules heated in a rocking furnace. Temperatures were determined to an estimated accuracy of 0.5°C with a Pt/Pt-10 pct Rh thermo-

Jan 1, 1963

By J. H. Hamilton, J. R. Lewis, J. H. Dismant, W. M. Fassell

RECENTLY this laboratory undertook the task of preparing some low carbon metallic cobalt by the carbon reduction of precipitated cobalt oxides. The oxides came in two lots and had the compositions given in Table I. Industrially, cobalt rondels&apos; are made by the carbon reduction of cobalt oxide in small reverberatory furnaces at temperatures near but not above 1050 °C. This is a slow and tedious small batch process but does give cobalt metal which is low in carbon (1 pct C). Inasmuch as these cobalt oxides were relatively low in copper and iron it was decided to reduce them with petroleum carbon in a small three-phase electric arc furnace of about 3 to 5 Ib of metal capacity. It was hoped such a procedure would save considerable time and perhaps also indicate an improved commercially feasible process. The furnace was preheated by using small pieces of carbon electrodes to maintain the arc until a temperature of 1500°C was reached. The broken pieces of electrodes were then removed and 500 g of the cobalt oxides and 60 to 100 g of petroleum coke added. At the end of the reduction reaction, a high lime flux was added to the furnace to facilitate the removal of sulphur. Due to the fineness of the cobalt oxide powder used and also to the presence of chlorides there was considerable dust lost in charging the furnace. This was overcome by preparing briquettes composed of the cobalt oxides, charcoal, and a little bentonite to serve as a binder. The results obtained are summarized in Table 11, which shows that the cobalt metal produced in the arc furnace was high in carbon varying from 2.5 to 3.5 pct. This, of course, is much too high. For certain uses, such as in the preparation of permanent magnets, the carbon content of cobalt must be low. It was necessary therefore to find an effective method of reducing the carbon content of the cobalt that had been prepared in the arc furnace. Van Arkel3 recommends the use of Co2O3 as a means of removing carbon from cobalt. Experiments by the authors indicate that carbon is removed with difficulty by this method. Other methods used, including lancing of the molten high carbon cobalt with a jet of oxygen, proved to be ineffective. The method finally used makes use of the fact that cobalt metal is decarburized by carbon dioxide at the temperature of the molten metal. Two methods were used: 1—carbon dioxide was bubbled up through the molten cobalt, and 2— molten cobalt was maintained in a carbon dioxide atmosphere. In the first method the gas was introduced below the surface of the molten metal by means of a quartz tube. A high frequency induction furnace was used to keep the cobalt molten in both of these experiments. This kept the metal somewhat agitated and no doubt was an important factor in hastening the decarburization &apos;process by the second method. Both methods gave satisfactory results as shown in Table 111. An interesting observation in connection with this &apos;work was that a small sample of carburized cobalt metal could be decarburized by heating it with an acetylene torch adjusted to give an oxidizing flame. This may have been due to the presence of carbon dioxide in the products of combustion. Samples of molten high carbon steel were decarburized by the same method and it is suggested that nickel and perhaps manganese can be decarburized in a similar manner. Additional work, including rate studies and other theoretical aspects of this problem, is in progress in this laboratory.

Jan 1, 1953

By C. G. Dunn

The measurement of interfacial teusions or grain boundary energies in metals is an important metallurgical problem, especially since it bears on growth and nucleation processes. Statistical methods of measuring equilibrium grain boundary angles, which relate interfacial tensions, have been used by some investigators1&apos;2 but more direct methods would be preferred. A direct way, based on a simple extension of a successful method of growing single crystals of silicon ferrite to predetermined orientations in flat specimens,3 is to produce three-grain specimens in such a way that the equilibrium common grain boundary will be perpendicular to the surface of the specimen. The angles to be measured then appear as the grain boundary angles in the surface of the specimen. The method of producing a single crystal specimen with a predetermined orientation is basically the same as that employed by Yoshida and Fuji-wara4 in their work on aluminum wires. The specimen, prior to any single crystal transformation, must have a matrix which will support the growth of a crystal of the desired orientation. Growth may occur through exaggerated grain growth or, if the matrix is strained a critical amount. by normal recrystallization. In either case the matrix must have stability at the temperature used to effect the transformation, this stability appearing as a long induction period for exaggerated grain growth or for the formation of recrystallization nuclei. Additional control is gained by using a high temperature gradient through which the specimen is moved at a suitable rate. To obtain the desired orientation, the specimen is fed a short way into the furnace producing one or more crystals in the hot end. After the specimen is removed from the furnace, the orientation of a crystal is determined, so that this crystal may be reoriented by properly deforming a narrow piece of the matrix between the end crystal and the rest of the specimen. This part of the specimen in the case of silicon ferrite is preferably held at red heat during the reorienting process. Fig 1 shows a specimen which is ready to be transformed into a single crystal through growth of a reoriented "seed" crystal. When the method just described is applied to the production of a three-grain specimen two crystals are grown first side by side in one end, the specimen is then reversed and the third grain grown from the opposite end. A suitable group of grains each of different orientation is one where all three grains have the same crystallo-graphic plane in the plane of the specimen. Fig 2 shows a photograph of a three-grain group prepared as described. The notches are introduced in the open ends of the grain boundaries to anchor them during the final annealing operations which ultimately should bring the grain boundaries to the lowest energy configuration. Two-grain groups with different crystallographic planes in the plane of the specimen can be similarly prepared and treated. If the two grains have different surface (gas to metal) energies per unit area, the equilibrium condition leads to a curved grain boundary.* * This feature of the problem was pointed out by J. c. Fisher. References 1. Cyril Stanley Smith: Grains. Phases and Interfaces: An Interpretation of Microstructure. Trans. AIME 175, 15. Met. Tech. TP 2387, June 1948. 2. D. Harker and E. Parker: Grain Shape and Grain Growth. Trans. A.S.M. (194,5) 34, 156-195. 3. C. G. Dunn, A. Seddon, and R. Wylie: Unpublished Work, 1946-1947. 4. Takeo Fujiwara: A Method of Producing A Long Single-Crystal Wire of Aluminum with any Desired Crystallographic Axis. Jnl. of Sci. Horoshima Univ. A, (1939) 9, No. 3, 227.

Jan 1, 1950

By W. C. Ellis

IN an ingot of germanium solidified progressively from the bottom by a method&apos; devised by J. H. Scaff and H. C. Theuerer, examination discloses ex- IH. C. Torrey and C. A. Whitmer, Crystal Rectifiers. p. 364. 1948. New York. McGraw-Hill Pub. Co. tensive twin relationships. A slice taken about midway in a cylindrical ingot approximately 3/4 in. in diameter and 1 1/2 in. in length, after etching and polishing to delineate different orientations, is shown in fig. la. The orientations of the regions designated with letters were determined by Laue X-ray back-reflection methods and plotted on stereograms. The orientation relationships of the designated components were determined by comparing the values for the nine angles between the three respective cube poles of each orientation with the values calculated in a formal treatment of octahedral multiple twinning in cubic crystals. Germanium, diamond cubic in structure, has the octahedral twinning habit. I am indebted to K. H. Storks for the calculation of the angular relationships of cube poles in octahedral twinning to four orders. The set of values for the nine angles is distinctive of the order of twinning. Confirmation for a multiple twin relationship is obtained from the determined indices of the mirror planes. These exist for all orders of twinning through the third and for some of the fourth." If the orientations are not those for twinning, then the nine angles for the cube poles do not correspond in value and distribution to those formally calculated. Since all nine angles must correspond in values and distribution of values to the calculated ones, the Laue method with a precision of one or two degrees is adequate to establish or deny with confidence the existence of multiple twins. Regions of the same orientation can also frequently be identified by the optical reflections. For example, the narrow twin bands in A at 2: 00 o&apos;clock have orientation B1. The interesting twin relationships shown schematically in fig. lb were found for the section in fig. la. Most of this slice was made up of orientation, A, appearing in widely separated regions. Of the four possible first order twins of A, three were present in this slice and are designated by B with subscripts. Four second order twins of A are designated by C with subscripts. It is worth emphasizing that two of these, C, and C,, are second orders of A through the first order missing in this section. Two regions, designated by D with subscripts are third order twins of A. D2 is a sixth order twin of D,. All orientations found were ascribable to multiple twinning, as if the orientations in this section originated earlier in solidification from a single nucleus. The presence of extensive multiple twinning to- gether with the absence of other orientations appears to be a characteristic result in many instances of solidification of germanium. Fertile conditions for twinning probably exist in the array of atoms in the diamond cubic structure. The high order twins in the section shown, it is reasonable to presume, are the result of progressive octahedral twinning through several generations in the material freezing earlier. Some of these generations do not appear in this section, it is suggested, because their orientations with respect to the growth direction were unfavorable for survival. The extensive twinning is probably promoted during solidification by constraint imposed by volume increase, and to an irregular growth front. Twinning may also be due, in part, to the attempt of the solidifying region to attain the orientation most favorable to the growth direction (maximum thermal gradient). The nucleus for a twinned orientation could have its origin in a "stacking fault" on the close-packed octahedral plane. Further work is being done in which the course of twinning throughout an ingot is being studied. The results appear to be important in the general theory of solidification.

Jan 1, 1951

By S. R. Mitchell, M. C. Fuerstenau, A. M. Gaudin

The two principal attributes of a thickener pulp are its settling rate and the ultimate pulp density of the thickened mud. Testing for evaluation of thickening attributes of a pulp has usually been done batch-wise by placing the pulp in a one-liter glass graduated cylinder and noting the position of the boundary between clear liquor and mud as a function of time. Refinements in testing have included repulping a thickened mud to various dilutions and evaluating the settling rate on these various repulped muds. This is considered to make possible an estimate of the settling rate as a function of pulp density and therefore to pinpoint the slowest settling pulp which ought to be critical from the standpoint of thickener plant design. Finally, tests are sometimes made with model-size continuous thickeners of arbitrary size. In batch tests it is generally accepted that the behavior of a pulp is described by a curve such as the one shown in Fig. 1, in which the position of the boundary between clear liquor and mud (the mudline) is plotted against time. It has also been assumed that the initial settling rate (the slope of the line segment AB) is descriptive of the pulp and independent of the size and shape of the container. Where the settling rate is slower and clearly a function of time (portion CD of the settling curve), it has been assumed that the data are not of much use because of the intrusion of compacting phenomena. The next important datum is the height. PE, which is a measure of the so-called ultimate pulp density. This quantity is assumed to be characteristic of the pulp and independent of the container. When actual data are recorded, results are rarely exactly according to this theory and numerous deviations may be noted. For example, some pulps seem to require an appreciable delay before beginning to settle, as in line AF. This is spoken of as representing the need for an induction time for flocculation. It has seemed desirable to explore thickener data with a more sensitive charting tool than is afforded by the coordinates of Fig. 1. Instead of relating the position of the mudline to time, it has seemed desirable to relate the rate of descent of the mudline to time. This, in effect, amounts to charting the slope of the line in Fig. 1, or the derivative of its ordinates, against the same abscissas. Fig. 2 shows the new chart for the curve ABCDE of Fig. 1. When this new tool was applied to data obtained, for example, with sized clay pulps, astonishing differences appeared. Apparently the traditional tool conceals differences instead of revealing them, whereas the new method emphasizes them. It seems, also, that both charting methods have their uses. In this article attention is focused on the effects of pulp density and container height as they affect the settling behavior of flocculated suspensions of a sized kaolin. The thesis by M. C. Fuerstenau&apos; gives more details than this summary, as well as some information about the effect of other variables. Sized fractions of kaolin were used, supplied through the courtesy of S. C. Lyons of the Georgia Kaolin Co. Large batches were made by agitation in a flotation machine and in a glass jar equipped with a mixer. The settling vessels were 2, 4, and 6-in. diam glass cylinders of various heights. Pulp Dilution: The effects of pulp dilution on sedimentation behavior are shown in Figs. 3, 4, and 5. Fig. 3 shows data on pulps ranging from 2.44 to 16.7 pct solids initial pulp density, flocculated with Separan and charted in the traditional manner. At least two of the lines appear nearly straight in their early sections, but neither of the others does. Each of the curves in this figure includes a region labeled

Jan 1, 1960

By R. E. Reed-Hill, W. H. Hartt, W. A. Slippy

An unusual form of double kinking has been observed at the ends of {1121} twins in deformed zirconium. These kinks lie partly outside of the twin and partly inside. While they are undoubtedly closely associated with accommodating the twinning shear into the matrix, they are apparently closely related to other important aspects of twin growth. A mechanism is proposed for {1121} twin growth involving interactions between 1/3 (1120) dislocations in the bend planes and twinning dislocations. It is also shown that boundaries without long range strain fields develop at the tapered ends of the twins. The {1121} twins can, therefore, grow without forming high-energy noncoherent twin boundaries containing large numbers of closely spaced twinning dislocations. NUMEROUS investigators have indicated that slip is often closely associated with deformation twinning. An example is twin accommodation kinking,1-3 where dislocations form bend planes and permit accommodation of a twinning shear within the parent crystal. Another is the incorporation of slip dislocations into twins, as proposed by Sleeswyk and verbraak4 and Ishii and Kiho5 for iron and ß-tin, respectively, and observed in hcp metals by Price.6 In addition, it has been shown that shear discontinuities exist at the points of twin intersections in zinc,7 magnesium,8 titanium,9 ß-tin,10 and bismuth," where the continuity conditions for twin intersections, originally proposed by cahn,12 are not satisfied. A similar situation occurs for zig-zag (1121) twins in zirconium13 and ?-phase silver-aluminum alloys,14 where the twinning shears of the two component twins are not parallel. In all these latter cases additional deformation by slip is believed to accommodate the twinning shear discontinuity. The present paper is concerned with a newly observed aspect of the slip and twinning interrelation, in which two kinks, one inside the twin and the other external to the twin, are formed. These kinks, observed in conjunction with (1121) twinning in zirconium, form to accommodate the twinning shear. A model has been constructed explaining the growth and accommodation of (1121) twins in terms of these kinks. This mechanism may be significant since it is concerned with an important twin mode, which occurs not only in zirconium but also in titanium and hafnium. The practical significance of (1121) twinning has been adequately demonstrated. At 77° K the high ductility of zirconium containing a large number of grains unfavorably oriented for slip is primarily due to (1121) twinning.&apos;5 Also, (1121) twins nucleated at 77°K may grow during further deformation at room temperature. This growth can greatly increase the transverse ductility15 as well as produce large mechanical hysteresis effects.= EXPERIMENTAL PROCEDURE Arc-melted, sponge zirconium plate previously described17 was prestrained 0.65 pct at 77° K by cold-rolling to introduce {1121} twins into the structure. Tensile specimens were cut with axes normal to the plate rolling direction. These specimens were pulled in tension to near the point of failure in an Instron machine at room temperature at a cross-head speed of 2 x10-2 in. per min. This additional deformation caused growth of the twins nucleated by prestrain. Deformed specimens were then prepared for metallo-graphic examination. This included an anodizing treatment18 that made the surfaces sensitive to polarized light, permitting small lattice rotations to be revealed. EXPERIMENTAL RESULTS Nature of the Twin-Kink Band Structure. Fig. 1 is a photomicrograph of a typical specimen after prestrain at 77° K. The structure is characterized primarily by long, narrow, parallel sided (1121) twins which norma1ly traverse the entire grain. Fig. 2 shows several (1121) twins after additional straining at room temperature. These lie near the center of the polarized light photomicrograph and are inclined upward to the right. It is evident that this latter deformation has resulted in appreciable twin growth. The dark regions extending from the ends of these twins are accommodation kinks. The difference in reflected light intensity indicates the

Jan 1, 1969

By O. C. Ralston, F. Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of 1/2 to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles. The sign of the potential on the corona-emitting electrode makes little difference in the separation. An electrode usually emits negative corona somewhat more easily than it emits positive corona, as electrons are then the fundamental particles emitted. With a positive electrode the flow of electrons involved in positive corona discharge is onto the electrode from the ambient gas. Theory In the separator illustrated in fig. 1, the nonioniz-ing electrode is a rotating, nonconductive dielectric cylinder designated as B. The ions emitted by the corona electrode, or wire F, charge both the particles on the carrier electrode, or roll A, and the surface of the dielectric electrode B. Whereas the space between roll A and wire F contains ions, the space between electrode B and roll A is a pure static field free of ions. The dielectric electrode has been described by Bullock.1 However, the corona electrode, which Bullock uses for the purpose of charging only the dielectric electrode, is adapted here to also charge the particles on the carrier roll. In operation the ionic field from the corona electrode is balanced with the static field from the dielectric electrode. The ionic field charges the particle so that it adheres to the roll. The static field intensifies the discharge of the corona charge by interfacial conduction and permits the release of the particle. The ionic and static fields therefore have opposing effects.2 The values of both fields are adjusted so that the poor conductor will adhere and the good conductor will be released.

Jan 1, 1951