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By C. R. Sandberg, C. A. Connally, N. Stein

This paper describes the results of volumetric efficiency tests on oil well pumps handling gas oil mixtures. The work was performed in a large scale, above ground unit wherein test conditions could be accurately controlled and measured. The main variables studied were gas/oil ratio (including gas from solution and free gas mixed with oil), pump compression ratio, pump stroke length, pump speed, and clearance volume between the valves at their closest approach. Results are presented for two different pumps and for oils of two viscosities. Relatively small amounts of gas entering the pump resulted in large decreases in volumetric efficiency. Under conditions where the pump was operating at reduced efficiency because of the presence of gas, it was found that variation in the clearance volume between the standing and traveling valves had a considerable effect on pump efficiency level. This effect of the valve clearance volume was found to be significantly altered by the viscosity of the oil used in the tests. The effects on pump efficiency of the other variables studied were found to be relatively small over the range of conditions utilized. INTRODUCTION The production of oil by pumping is often hampered by low volumetric efficiency. A direct increase in lifting costs results from low volumetric efficiency. An indirect increase in lifting costs, probably greater than the direct increase, results from additional wear and tear on pumping equipment and from the down-time necessary for the repairs which can be traced to low-efficiency operation. Both increases in lifting costs tend to reduce economically recoverable oil. A number of different factors can contribute to low pump efficiency. A known basic cause of low efficiency is the presence of free gas in the pumped fluid. Pump volumetric efficiency is calculated only on the basis of liquid pumped and because any free gas pumped is discounted, this volume of free gas would represent a loss of pump efficiency. However, gas also causes a reduction in pump efficiency because it is a highly compressible fluid. It is known that pumps some- times "gas lock" because of excessive gas-to-liquid ratios in the pump barrel. Little is known of the role of gas compressibility in the intermediate case where the pump is operating at low efficiency. The opinion exists, however, that oil-well pumps tend to operate at higher efficiency with long stroke lengths at low speeds, but no quantitative studies of these pumping variables have been reported. It was believed that a much better understanding of the variables which control pump volumetric efficiency could be obtained and that possibly some suggestions as to the methods for increasing efficiency might be found from a study of the operation of pumps handling gas under closely controlled conditions. Previous investigators have studied the effects on pump efficiency of such factors as oil viscosity, oil temperature, slippage of oil. past pump plungers, pump submergence, valve size and spacing, pressure above pump plunger and fluid vapor pressure. However, none of these published investigations were conducted with pumps being subjected to large amounts of gas such as might be the case in a pumping well, nor did any of the investigations study the effect of variation in stroke length or pump speed. A large-scale teat unit was therefore constructed for studying the operation of pumps handling gas and for evaluating effects of such variables as pump stroke length and pump speed. PROCEDURE AND EQUIPMENT A schematic diagram of the pump testing equipment is given in Fig. 1. A 45-ft length of 6-in. casing is mounted vertically in a 65-ft tower. Sight ports are mounted in the casing at intervals near the location of the pump intake and the liquid level in the casing. These sight ports are fitted with Lucite windows sealed by neoprene "0" rings. The Lucite windows are machined to conform to the I.D. of the casing so that no obstruction to flow is present along the casing wall. The casing is fitted with a tubing head and 2-in. tubing is hung inside the casing. Pumps are seated in a shoe attached to the 2-in. tubing. A 1-in. polish rod is attacked directly to the pump without any intervening sucker rods. The top of the polish rod is attached to the weight carrier, which contains a number of weights to be used to force the polish rod in against tubing pressure on the down-stroke. This is necessary because a long string of sucker

Jan 1, 1953

By E. T. Turkdogan, Klaus Schwerdtfeger

OelSEN and Maetz1 detected some 20 years ago the existence of a miscibility gap in iron oxide-CaO-P2O5 slags melted in iron crucibles at about 1400°C. Because of the importance of this system for the dephos-phorization of steel in the basic Bessemer process, equilibria between liquid iron and selected iron oxide-CaO-P2Q slags have been measured since by numerous investigators.2-5 When in equilibrium with metallic iron, the iron oxide of the slag is present mainly as FeO. In connection with oxygen-blowing steelmaking processes, it is useful to know the phase relations in the slag system at higher oxygen pressure, when major parts of the iron oxide are present as Fe2O3. This problem was investigated by Turkdogan and Bills7 by equilibrating the oxide mixtures contained in platinum crucibles with CO2-CO mixtures at 1550°C. It was found that increasing the Fe2O3 content decreases the composition range of the miscibility gap strongly so that the miscibility gap has almost disappeared at pco2/pco = 75. This result was refuted by the careful work of Olette et a1.,''' who equilibrated their slags with controlled Ha-H2-Ar gas mixtures. Their equilibrium measurements, at 1600°C and at oxygen pressures of 5 x 10"* and 10"5 atm, showed that the oxidation state of the iron has almost no influence on the formation of the miscibility gap. The present experiments were undertaken to check the previous results of Turkdogan and Bills. The experiments were performed at 1625°C in the strongly oxidizing atmosphere of air (PO2 = 0.20 atm) for which no experimental data are available. About 10 g of slag were melted in platinum crucibles and held at constant temperature for 1 hr. After equilibration, the crucible was rapidly pulled out of the furnace and cooled in air. The platinum crucible was removed from the sample. The two slag layers were carefully separated with a small diamond disc, and the surface of the top layer, which may have changed its oxidation state during cooling, was removed. The slags were crushed and analyzed chemically for CaO, P2O5, Fe2+, and Fetotal. The starting mixtures were prepared by sintering the desired amounts of reagent-grade 2CaO . P2O5 - H2O, CaCO3, and Fe2O3. Sintering and subsequent crushing were done three times to ensure homogenization. Molybdenum wire resistance heating was used. The furnace was provided with a recrystallized alumina reaction tube which was left open to air at the top. The temperature was controlled electronically. The reported temperature was measured with a Pt/Pt-10 pct Rh thermocouple and is estimated to be accurate within +5°C. The composition of the equilibrated melts is given in Table I. For the graphical illustration of these quaternary slags the type of projection suggested by Trömel and Fritze10 was used. In this representation, Fig. 1, the composition point of a mixture within the tetrahedron Fe2O3-CaO-P2O5-FeO is projected into the Fe2O3-CaO-P2O5, triangle (triangle I) so that the direction of projection is parallel to the side FeO-Fe2O3, and into the triangle Fe2O3-P2O,-Fe0 (triangle 11) so that the direction of projection is parallel to the side CaO-P2O5, of the tetrahedron. The projected point has the coordinates wt pct CaO, wt pct P205, and wt pct (FeO + Fe2O3) in triangle I and wt pct FeO, wt pct Fe2O3, and wt pct (CaO + PzO5) in triangle 11. Both triangles are turned into the same plane around the Fe203-P20, side of the tetrahedron. An illustration of the projection of a quaternary point in the present system is shown in Fig. 1. The advantage of this type of projection is that all four components for an equilibrium curve can be read directly from the diagram. The present results are shown graphically in Fig. 2. The curves depicting the miscibility gap are dashed in parts where no experimental points were obtained. The composition range covered by the miscibility gap

Jan 1, 1968

By E. A. Almond

An attempt is made to explain the effect of stress on strain aging by examining the mechanism of yielding for a group of aged dislocations. The experimental results on which the theory is based indicate that a linear relationship develops between the aging stress and the discontinuous yield effect in a low carbon steel THE discontinuous yield effect that occurs in bcc metals after strain aging is usually explained by the interaction of interstitial atoms with individual dislocations. Attempts have been made to interpret the kinetics of strain aging in terms of interstitial segregation to nonrandom groups of dislocations1-3 but apart from Li's4 work little or no effort has been made to examine the effect of groups of aged dislocations on mechanical properties. It appears likely that such groups can be stabilized if a positive load is maintained on the specimen during aging5 and, furthermore, that the enhanced strain aging effect associated with aging under load might be due to the stability of these aged groups. The effects associated with this latter phenomenon have been described by Almond and Hull, Ref. 5, Figs. 2 and 3, and it is found that the upper yield stress, the lower yield stress, and the yield point elongation are increased by aging under load. The yield point elongation reaches a maximum value but the enhanced effect persists in the upper and lower yield stress values even after extended aging treatments when the general level of the flow stress curve rises. The flow stress, as measured at 8.5 pct total strain, however, is independent of aging stress. Almond and Hull5 showed that it was unlikely that the differences in mechanical properties could be caused by stress enhanced diffusion and they suggested that the effect was in some way associated with the different dislocation distributions that are obtained when specimens are aged with and without an applied stress. At that time no explanation was offered for the strengthening effect produced by stabilized dislocation distributions but additional tests have been performed to establish a quantitative relationship between aging stress and mechanical properties, and also to examine more closely the effect of varying the procedure for applying the aging stress. EXPERIMENTAL The material used was an iron wire containing 0.015 wt pct C, 0.002 wt pct N, and 0.006 wt pct 0. Tensile specimens with a 1 cm gage length and 0.08 cm diam were annealed at 850°C for 1 hr in vacuum to establish a grain diameter of 0.032 mm and then aged at 200°C for 24 hr. After this treatment the amount of carbon left in solution would be less than 10-4 wt pct, and ni- as aging time is increased. It is suggested that this observation, and effects that arise from varying the method of applying the aging stress, can be explained by a strengthening mechanism whereby dislocations are more difficult to move when they are aged in piled-up groups. trogen would be the main cause of strain aging. Tensile tests were performed in a hard beam machine at a constant crosshead speed of 0.02 cm per min and the specimen chamber was immersed in a temperature controlled silicone oil bath at 32" * 0.05"C. RESULTS All specimens were prestrained 5 pct before aging under stress and the results in Figs. 1 to 5 show the effect of aging time and aging stress on the following parameters ?UY = auy — ?F(5); i.e., the difference between the upper yield stress after aging,?uy, and the flow stress after prestraining 5 pct, ?f(5). ?LY = sly —sf(5); the difference between the lower yield stress after aging, ojy, and the flow stress after prestraining 5 pct. s8.5 = the flow stress at 8.5 pct total strain after aging at 5 pct strain. Varying the Loading Procedure. Three variations in the procedure for applying the aging stress were examined; i) After prestraining, the specimen was unloaded to a stress of 18 kg mm-2, aged at that stress, and then tested. ii) After prestraining, the specimen was unloaded to 2 kg mm-" then reloaded to 18 kg mm-', aged at that stress, and tested. iii) After prestraining, the specimen was unloaded to 18 kg mm-', aged at that stress, then unloaded to 2 kg mm- before testing. Specimens were unloaded or reloaded by decoupling a clutch in the drive transmission of the tensile machine. This enabled the crosshead to be driven manu-

Jan 1, 1970

By B. D. Cullity

AS methods for measuring fiber textures become more exact, it becomes justifiable to scrutinize an observed pole-density curve for evidence of minor texture components. These are disclosed by minor maxima or abnormally broad major maxima. One possible source of these minor components is twinning of the main component. In cubic metals and alloys, there are two kinds of twins: 1) Annealing twins in face-centered cubic metals. These are reflection twins on {Ill), and they can be expected to be present in recrystallization textures. 2) Deformation twins in body-centered cubic metals. These are shear twins on (112). Although usually formed only by impact, they might conceivably be present in the deformation texture of severely cold-drawn wire. Fortunately, both kinds of twinning lead to the same orientation relationships. It thus becomes possible to prepare a single list of angles between various planes in parent crystal and twin, which is helpful in examining pole-density curves for evidence of twinning in any cubic metal or alloy. Such a list of interplanar angles is given in Table I. This table consists of three parts, corresponding to the three major texture components—<100>, <110>, and <111>-most commonly found in the fiber textures of cubic metals. The table lists the angle between the pole of {hkl}, in either the parent crystal P or the twin T, and the fiber axis <uvu>. The crystals with <uvw> parallel to the wire axis are here

Jan 1, 1959

By Jack L. Taylor

Single crystals of tungsten grown from powder -metallurgy swaged rod by high-temperative annealing were deformed in tetzsion at temperatures from 2500 to 5000 OF. Orientation of specittzen tensile axis, strained ratrix, and defortnation bands was determined optically by reflections from {110} etch pits. Slip traces meve analyzed and slip directiorz determined. Results indicate that {110}(111) , {112){111}. and {123}{111} type slip occur in tungsten over the terpe,atuve rutge investigated. Slip is orientation-dependent occuvring on tCuzt cowzbitzation oj slip plane and direction which has the highest critical resolved shear stvess. Overshooting appears to be a general occurrence between 2500&apos; and 5000°F. Dejornatiotz bands show rotation in a directiorz opposite to the yotation of tire tensile axis. DEFORMATION in bcc metals has been reviewed by Maddin and Chen,&apos; Keh and eissman,&apos; and most recently by Nabarro, Basinski, and olt. From these reviews it is apparent that some disagreement exists concerning the crystallography of plastic deformation in bcc metals. There is evidence of noncrystallo-graphic slip, the crystal slipping on or near a noncrys-tallographic plane in the (111) zone for which the resolved shear stress is greatest. There is also evidence to indicate that crystallographic slip occurs in the planes of the same zone. On the other hand, there is agreement that the close-packed direction ( 111) is the slip direction in bcc metals. Further, in pure bcc metals4 and alloys the operative crystallographic slip systems are strongly dependent on temperature. Both crystallographic and noncrystallographic slip have been reportede8 in tungsten, a group VIA bcc metal. The number of slip families which operate in the case of crystallographic slip, however, has been in question. The earliest study by oucher&apos; of single-crystal tungsten tested at temperatures of 1800 to 5000°F led to the conclusion that only {112)( 111) type slip operated. Raymond and eumann recently reached the same conclusion studying deformation by rolling of plasma-flame single crystals at 1800°F; however, only [loo] and [110] orientations were studied. Work at high temperatures by Leber and Pughs on tungsten and Chen and Maddin9 on molybdenum suggests that conjugate slip on nonparallel (110) planes may account for the slip on (112) and (123) planes found by others working with bcc metals. The present paper presents evidence of three families or modes of slip in tungsten in the temperature EXPERIMENTAL PROCEDURE Material. Standard microtensile specimens, 0.160 in. diam by 0.640 in. gage length, were ground from commercial powder-metallurgy swaged tungsten rod, type MK. Specimens were heated for 10 min at 5150°F or 6 hr at 5400°F in vacuum of 1 x 105 Torr or less to produce single crystals. At the lower temperature an average of two out of seven specimens heated in a group developed single crystals throughout the specimen length as shown in Fig. 1, the rest remaining wholly poly crystalline. At the higher temperature, three or four out of seven specimens became single crystal. Other than to note that Laue X-ray photographs generally showed sharp, well-defined spots, no attempt was made to assess crystal perfection or measure dislocation density. Two tungsten single crystals grown from the melt by the plasma-arc process were also used for this study.

Jan 1, 1967

By J. B. Scuffham, G. Eggett, W. R. Hopkins

With solvent extraction now being accepted as a major method for recovering copper from leach liquors, the authors&apos; company decided that in tankhouse design full advantage was not being taken of the benefits available from sol- vent extraction produced electrolytes. Consequently, a major development program was undertaken to examine means of operating such tankhouses with current densities in excess of current electrowinning practice. Techniques investigated included high circulation of liquors, current reversal and the application of ultrasonics. At the same time there was a necessity for improving the quality of cathodes produced from electrolytes of high free acid content. The application of anodes which are capable of reducing or eliminating the lead content of cathodes is described in the paper. The other problem area in eletrowinning from solvent extraction produced electrolytes is the production of a higher degree of acid mist. Techniques for alleviating this problem are described bearing in mind their possible effects on the solvent extraction section of the plant.

Jan 1, 1973

By L. J. M. Smits

A theoretical equation is developed describing membrane potentials of shaly sands as a function of the cation-exchange capacity per unit pore volume of the rock and saturating water salinity. This equation is based on the same simple physical model as that employed earlier7 describing the electrical conductivity of shaly sands. Experiments conducted with NaCl solutions showed that the equation is obeyed, except in the case of saturated salt solutions where minor deviations were observed. A possible explanation is given for this discrepancy. As the clay content and the porosity of shales may vary appreciably, shale membrane potentials also vary. It was found that membrane potentials of shales can be calculated accurately with the aid of the same theory. Consequently, changes in membrane potentials can be accounted for by simple measurement of cation-exchange capacities per unit pore volume of both shales and shaly sands. Charts are given to facilitate interpretation of the electrochemical part of the SP in terms of cation-exchange capacities and the salinities of mud filtrate and formation water. INTRODUCTION A spontaneous potential (SP) log is a record of the way in which the electrical potential of a sonde varies as it passes down a borehole. Such variations frequently reflect rock texture, e.g., permeable beds intercalated in an impermeable series often are indicated by a sharp change in potential. Nowadays it is recognized that SP logs may be interpreted in terms of formation-water salinity and formation shaliness. The four sources of the SP are illustrated in Fig. 1. El and E4 represent streaming potentials generated by the flow of mud filtrate through mud cake opposite permeable formations and through shale, respectively. An extensive review of the literature on the evaluation of these streaming potentials is given by Lynchl and will not be discussed here. The remaining part of the SP generally is called the electrochemical potential, which is divided into two parts: a membrane potential across the shale (E3, Fig. 1) and a membrane potential in the permeable sand at the diffusion boundary between formation water and mud filtrate (E2, Fig. 1). It was found by wyllie2 that the membrane potential across the shale, E3, is the most important contribution to the electrochemical potential, the shale acting as a semi permeable membrane. When the sand is clean it does not influence the diffusion process, so E2 equals the value of the so-called liquid-liquid junction potential observed when the two solutions diffuse freely into each other. When the sand contains clay, however, this interferes with the diffusion process and affects the diffusion potential generated. The greater the proportion of clay, the stronger this effect will be. Wyllie,3 Doll4 and Poupon et al.5 took this effect into account theoretically, starting from a physical

Jan 1, 1969

By G. S. Cole

The temperature has been measured ahead of stationary solid-liquid interfaces under conditions approximating luzidirectional heat flow and therefore unidirectional solidification. Natural convection flow patterns may be deduced from the temperature distributions , temperature fluctuations, and shape of the interface. Fluid flow increases with the height and the rate of heat transfev through the interface and this is further manifested by a deviation of the interface from aflat vertical plane. The influence of fluid flow on solute inhomogeneity during alloy crystal growth can be inferred from the observed temperature distributions. A buoyancy force exists in the liquid ahead of a vertical solid-liquid interface, caused by a difference in density between cold fluid near the interface and warmer fluid in the bulk liquid. When the viscous and inertia forces in the melt exceed this buoyancy force, a flow of fluid takes place, termed natural or free thermal convection. Natural convection in purely liquid systems has been extensively studied for many years. 1"u On the other hand, fluid flow during horizontal crystal growth has oniy recently been the subject of experimental investigation."-25 The requirements for horizontal crystal growth differ from other heat flow systems. The small aspect ratio (ratio of height of cold wall to length of fluid) has never been considered. The uniform furnace gradient which supplies heat radially (and not necessarily symmetrically) differs from previous boundary conditions of uniform heat flux at the cold and hot ends. And most important of all an isothermal s/l interface is present which can adjust its shape and position to conform to heat and fluid flow. All of these boundary conditions involve complexities which cannot be readily solved analytically. Preliminary observation has demonstrated the penera1 shape of the natural convective flow pattern in transparent media.20&apos;24&apos;25 The flow is circulatory, directed toward the interface at the surface of the liquid, down and away from the interface at the bottom, and then up at the hot end of the melt. During crystal growth such a flow may interact with the solute boundary layer at the s/l interface to affect solute incorporation.M&apos;1B|28&apos;i!T Evidence has also been presented recently to show that thermal convective flow will affect the structure of ca~tin~s.~~-~~ The rate of heat transfer (conduction plus convection) in a given fluid system is a function of the temperature difference between the hot end of the liquid and the s/l interface and the height of the interface. At the lowest values of these variables* all heat is *It has been shown&apos; that adverse temperature gradients as low as O.OOS°C oer cm are sufficient to cause convection. transferred by conduction. When the temperature difference or interface height are increased, laminar fluid flow commences and heat transport takes place by laminar convection as well as by conduction; turbulent heat transfer takes place at higher values of these variables. In the transition region between laminar and turbulent flow, boundary layer separation takes place; fluctuations in temperature are also noted and increase in amplitude and frequency as turbulence becomes dominant. In this paper, fluid flow patterns in the melt ahead of a stationary interface are deduced from observations of temperature distribution and fluctuations, heat flow rate, and interface shape. The fluid flow ahead of advancing interfaces and the effect of such flow on solute incorporation may be inferred from these measurements on stationary interfaces. Observations during enforced fluid motion will also be considered. EXPERIMENTAL PROCEDURE The metal was contained in a lava boat 10 cm in length, 1+ cm in width, and 2 cm in height, as shown in Fig. 1. A water-cooled, molybdenum block heat-sink is at one end of the boat; surrounding this assembly is a slotted stainless-steel tube noninductively wound with a nichrome heating element. Temperature was measured by 38-gage Chrome1 vs Alumel thermocouples sheathed in 0.05-cm-diam graphite-coated stainless-steel tubing, which were moved longitudinally and vertically through the melt by means of a two-dimensional motorized micrometer stage. In some experiments the thermocouple junction was exposed, but in the majority of experiments the junction was welded to the sheath tip; no significant difference

Jan 1, 1968

By H. T. Green, R. M. Brick

True stress-strain data on alloys of pure iron with up to 2.4 pct Al were obtained in the temperature range +100° to —185°C. Alumi-num was found to reduce yield and flow stresses of iron at low temperatures but to have little or no effect on ductility. The effects of temperature and composition on strain hardening are discussed. SEVERAL independent studies of the behavior of high purity iron binary alloys at low temperatures are now in progress in attempts to evaluate systematically the variables affecting the low temperature brittleness of ferritic steels. This paper reports the results of one such investigation in which the tensile properties of aluminum and aluminum plus silicon ferrites were measured from 100" to —192°C. True stress-natural strain data have been obtained in order to evaluate as many as possible of the parameters which describe the behavior of the materials involved. In comparable studies at the National Physical Laboratory in England, iron and iron alloys of high purity have been produced&apos; and tested at subat-mospheric temperatures.&apos; True stress-natural strain curves were obtained there also. The purest iron contained 0.0025 pct C and 0.001 pct O and N. Even this, as normalized at 950°C following hot rolling, showed little ductility at -196°C. The grain size was ASTM No. 3, and the room-temperature yield strength was 17,800 psi (which seems too high for pure iron). Some of the NPL irons contained considerably more oxygen and demonstrated intergran-ular fracture at —196°C. The authors2 carefully differentiated between intergranular fractures associated with excessive oxygen content and transcrys-talline cleavage with little ductility encountered at —196°C in the purer material. The cleavage stress was half again as great as that associated with inter-granular fracture. Test Material, Preparation, and Procedures Of a number of Fe-A1 alloys produced, eight were considered to be sufficiently pure for testing. Partial chemical analyses (Table I), low observed yield points, and high ductilities indicate these alloys to be comparatively pure for vacuum-melted irons of sizable ingots, 5 Ib or more. To produce the binary Fe-A1 alloys, electrolytic iron was melted in air, cast into slabs, and rolled to strips 0.010 in. thick. These strips, joined into a continuous ribbon and wound into 2 1/2 in. diameter spools, were subjected for four weeks to a moving atmosphere of purified dry hydrogen in a stainless-steel tube at 1050" to 1150°C. Charges of these spools were melted in beryllia crucibles under good vacuums (1 micron), and aluminum (99.97 pct Al) was added to the melts. Compositions of these alloys are recorded in Table I. The ingots were hot forged and then cold rolled at least 65 pct to 3/8 in. rods which were vacuum annealed to the desired grain size, approximately ASTM No. 4, prior to machining into tensile test bars. All tensile specimens had gage sections 1 in. long, with a fillet of 1.5 in. radius to the shoulder. Gage diameters were 0.250 in, except for a few rods where additional cold work required use of a 0.200 in. gage section. After machining, 0.002 in. was removed from the gage diameter using 240, 400, and 600-grit metallo-graphic papers. The final polish with 600 grit left the fine scratches running in the longitudinal direction. By this means, surface metal strained during machining was removed. A few specimens heat treated after machining were similarly reduced 0.004 in. to remove any material affected chemically by the atmosphere during heat treatments, as is discussed in a later section. Tensile tests of the eight alloys at constant temperatures from +100° to —185°C were performed in apparatus which has been described." The essentials include a double-walled insulated metal vessel which contained the liquid heat-transfer medium surrounding the test specimen. A constant temperature was maintained by means of a pyrometer which regulated the pressure of dry air driving liquid air through a copper coil. Temperature variation was less than ±2°C during a specific test. For axial straining, two lengths of case-hardened chain, terminating in simple shackles, loaded the specimen through threaded grips. The lower grip bar passed through a hole in the bottom of the test vessel to which it was joined by a thin-walled

Jan 1, 1955

By L. A. Bromley, A. W. Petersen

The van Arkel-deBoer method for producing ductile titanium by thermal decomposition of Til, vapor and deposition on an electrically heated filament is modified by film boiling Til liquid on a heated filament, resulting in similar titanium deposition on the filament and liberation of gaseous iodine. The deposition rate is higher and the energy requirement smaller than in the van Arkel process. Many problems must be solved before the process is commercially feasible. TITANIUM of 99.9 pct purity, called ductile titanium, has been produced by a modification of the van Arkel-deBoer&apos; method. In the van Arkel-deBoer method, an electrically heated wire is suspended from two electrodes, which are placed in a container holding TiI, vapor at a low&apos; vapor pressure (usually <5 mm Hg). The vapor diffuses to the hot wire, usually maintained at 1100" to 1600°C,&apos; and decomposes according to the reaction liberating gaseous atomic iodine and depositing solid crystalline titanium on the wire. Estimations based on the data of Runnalls and Pidgeon,&apos; indicate that the rate-control ling step is the diffusion of atomic iodine away from the wire. There appears to be nearly thermodynamic equilibrium at the wire with TiI, and iodine as the main gaseous species. TiI, is almost certainly an important gaseous species in the cooler regions.&apos; The liberated iodine diffuses to a heated source of crude titanium and reacts to form more TiI, vapor, which again diffuses to the hot wire and completes the cyclic process. The foregoing process may be modified by suspending the hot wire in liquid TiI,, instead of the vapor, and obtaining film boiling. This type of boiling is characterized by the formation of a continuous film of vapor over the wire surface. Since only vapor contacts the wire sul.face, the temperature of this surface may be raised as high as desirable, within the limit of mechanical strength requirements for the wire. By properly adjusting the input voltage. the temperature of the wire may be maintained above U0C"C; and by evacuating the vessel holding the liquid TiI, and maintaining a suitable condenser temperature, the vapor pressure of TiI, may be held low. Thus, the conditions of operation of the van Arkel-deBoer method may be approximated with film boiling; and hence, it is postulated that ductile titanium may be produced by this method. Preparation of Til, There are many methods available for the preparation of TiI,; that used in this research was prepared by the direct reaction of titanium sponge in controlled amounts with liquid iodine. Although no difficulty was encountered with this reaction, it has since been pointed out that this method is sometimes dangerous and should be used with caution. The resulting TiI, was purified by distillation. First Film Boiling Experiments Apparatus: The apparatus shown in Fig. 1 was used for film boiling TiI, on short wire filaments. The current to the filament was supplied through a bank of three 5 kva transformers connected in parallel. The current was controlled by adjusting the voltage over a 0 to 67.5 v range with a 7 kva variable transformer on the low voltage side of the bank of transformers. The current and voltage were measured by Weston meters. The sealed-in-glass tungsten electrodes were hard-soldered to the filament for the film boiling of TiI,. The bottom part of the reactor, containing TiI,, was wrapped with ni-chrome heating wires to maintain the TiI, in the liquid state. An ice or liquid nitrogen trap, for solidifying I, vapor and any TiI, not condensed, was attached to the low pressure side of the air-cooled condenser. A Megavac vacuum pump was used. Procedure: A 0.010 in. diam tungsten filament was hard-soldered to the tungsten electrodes. TiI, was melted (mp 156°C) and poured into the reactor chamber; the top of the reactor chamber, containing the electrodes, was replaced. Freezing of the TiI, was prevented by controlling the current to the ni-chrome wires wrapped around the reactor with a 1 kva variable transformer. The mechanical vacuum pump was started and the system evacuated to about 2 mm Hg TiI, vapor pressure. The current to the filament was turned on and the impressed voltage slowly increased with the variable transformer. A sudden drop in current at nearly constant im-

Jan 1, 1957

By Carl E. Swartz

For many years kettles used in the melting and refining of lead and other nonferrous metals and alloys have been made of cast iron. The logic of this probably lies in the fact that cast iron has been known as a material of construction for vessels of this type much longer than steel, and satisfactory fabrication from it has been more easily accomplished and better understood. As the capacity of lead refineries has increased, it has been only natural to increase the size of kettles. Today kettles of 150 to 250 tons are not uncommon. As the size of the kettles increased and better shapes were designed, the uniformity of material of construction became more important. Records kept over comparatively long periods of time have shown that the length of service of kettles has not been uniform. Many causes contribute to this and the importance of each has not yet been evaluated. Kettle design, kettle setting, method of firing and material of construction have been changed from time to time to obtain better service, but the variation in length of service is still great. A kettle may fail during the first few heats or may last through more than one thousand heats. The purpose of this article is not to present the conclusions of a finished piece of research on kettle manufacture and use, but to present a series of observations made over considerable time in the hope that others will publish data and that all may be correlated into a logical scheme which will result in better service and longer kettle life.

Jan 1, 1931

By W. H. Basssett

THE amount of oxygen present in refined copper bears an important relation to the effects of various impurities on physical properties of copper, as well as the effects of reducing gases at higher temperatures. It seems fitting at this time, when the effects of reducing gases on copper are being discussed, to describe methods that have proved satisfactory for the determination of oxygen and sulfur, and to present some results obtained by investigation of these methods in the authors&apos; laboratory. The procedure for the determination of sulfur is closely interrelated with that for oxygen and has, therefore, been included. It was first proposed by Hamper that oxides in copper could be accurately determined by the loss in weight sustained by finely divided copper when reduced at red heat in pure hydrogen, or by the weight of water produced. Hampe&apos;s method was later modified by Archbutt,2 who established the accuracy of the method and demonstrated that equally accurate results were obtained by noting the loss in weight or by weighing the water formed. The determination of oxygen by heating in carbon monoxide has been proposed by West.3 In our hands this method has given slightly lower results than obtained by heating in hydrogen.

Jan 2, 1926

By Stewart L. Toleman, Robert H. Hafner, Irvin R. Kramer

In his paper on the calculation of harden-ability from chemical composition, Gross-mannl discussed the effect of most of the alloying elements used commercially. The purpose of the work reported in this paper was to determine the effect of several other elements on hardenability—arsenic, antimony, beryllium, cobalt, columbium, germanium, tellurium, tin, aluminum, and titanium—and to extend the range of composition of some of the elements studied by Grossmann—chromium, copper, manganese, molybdenum, nickel and silicon. Experimental Methods To determine the effect on hardenability, suitable amounts of the alloying elements were added to experimental heats and the hardenability determined by means of end-quenched hardenability specimens. The steels were melted in a high-frequency induction furnace with a basic crucible, using ingot iron as a base for some of the heats and S.A.E. 1015 for others. The alloying additions were made as ferroalloys or as metal, depending on the alloying element. Hundred-pound heats were split and poured into square, tapered, cast-iron ingot molds with hot tops. Aluminum was not used as a deoxidizer in most of the heats. The ingots were homogenized for 12 hr. at 1260°C. (23oo°F.) and forged into rounds of I½ -in. diameter. These bars were normalized twice from 840°C. (I55o°F.) before machining into Jominy bars. mined in most Cases by samples taken from the end-quench hardenability spedmen. AS suggested by Crafts,2 acid-soluble (8

Jan 1, 1944

By R. H. Doremus

From measurements of carbide precipitation rates in a iron it was concluded that the carbides nucleated on dislocations in both strained and unstrained samples, except for the latter at lower temperatures and higher carbon concentrations, where there were more muclei than could form on the dislocations. The equation of Cottrell and Bilby for the segregation of atoms to dislocations was found to be inapplicable to this system. No satisfactory theory for the growth process is available. A study of the rate at which a second phase separates from solid solution can frequently reveal much about the mechanism of separation. There are still many features of the precipitation of carbon from a iron that are not understood, although this system has been examined extensively. To provide more insight into the mechanism of carbide precipitation in a iron, rates of this process were measured at different temperatures, carbon concentrations, and densities of dislocations in the iron. The concentra- tion of carbon in solution was followed from the height of the internal-friction peak; this height is directly proportional to the amount of carbon in solution and is not affected by the growing carbide particles. In this paper these rates are compared with those found by earlier investigators, and the mechanism of precipitation is discussed in light of these results as well as two earlier studies1, 2 and the electron microscopic work reported in the preceding paper. EXPERIMENTAL The amount of carbon in solution was followed by

Jan 1, 1961

By William Blauvelt

Tun technical and engineering problems in the manufacture of coke are today the problems of the byproduct oven. Except in a few special localities, practically no beehive ovens have been built in the United States for the last 5 or 6 years except as renewals of old plants, and during these years the total number of beehive ovens in existence has been steadily falling. On the other hand, the number of byproduct ovens has increased from 4624 in 1911 to a total of about 7660 in operation at the end of 1917; with 2800 building, this makes a total of about 10,460 which will be in operation in 1918, or shortly thereafter. Preliminary Government estimates place the total production of coke for 1917 at 56,600,000 tons, the largest tonnage in the history of the industry. Of this 34,000,000 tons or 60 per cent. was beehive, and 22,-600,000 tons, or 40 per cent. was byproduct coke. Some time in 1918 the production of byproduct coke should pass the beehive output, and when the byproduct ovens now building are completed the total byproduct capacity will be about 40,000,000 tons of coke per. annum, which is over 70 per cent. of the record-breaking total coke production of 1917. The reasons for these changes in the coking industry are familiar to all of us, and need not be discussed here.

Jan 3, 1918

By Robert H. Hafner, Irvin R. Kramer, Stewart L. Toleman

In his paper on the calculation of harden-ability from chemical composition, Gross-mannl discussed the effect of most of the alloying elements used commercially. The purpose of the work reported in this paper was to determine the effect of several other elements on hardenability—arsenic, antimony, beryllium, cobalt, columbium, germanium, tellurium, tin, aluminum, and titanium—and to extend the range of composition of some of the elements studied by Grossmann—chromium, copper, manganese, molybdenum, nickel and silicon. Experimental Methods To determine the effect on hardenability, suitable amounts of the alloying elements were added to experimental heats and the hardenability determined by means of end-quenched hardenability specimens. The steels were melted in a high-frequency induction furnace with a basic crucible, using ingot iron as a base for some of the heats and S.A.E. 1015 for others. The alloying additions were made as ferroalloys or as metal, depending on the alloying element. Hundred-pound heats were split and poured into square, tapered, cast-iron ingot molds with hot tops. Aluminum was not used as a deoxidizer in most of the heats. The ingots were homogenized for 12 hr. at 1260°C. (23oo°F.) and forged into rounds of I½ -in. diameter. These bars were normalized twice from 840°C. (I55o°F.) before machining into Jominy bars. mined in most Cases by samples taken from the end-quench hardenability spedmen. AS suggested by Crafts,2 acid-soluble (8

Jan 1, 1944

By Yinchang Wang

1. INTRODUCTION 1. Subject, and Scope The formation of the oxidized ores of zinc has been recognized as a subject of great importance in economic geology. For many years these ores have been much sought, partly because they are more desirable for metallurgical treatment and partly because they are apt to be freer from gangue than is the sulphide of zinc. Up to very recent years the oxidized ores were the principal source of the metal and at present they still furnish a large portion of the commercial production. . The oxidized ores of zinc include six minerals, as shown in the-following table

Jan 9, 1915

By A. W. H. Morris, E. A. Steigerwald

The jatzgue beizazriov oj Mietal matrix co))zpos~tes in tension -lensiom loading has been imestigated as a junction of Dolume fraclion veinfovcelnent using the model systems of a silver matrix reinforced with contlnuous or dzscontztinuous aligned tungsten jilamenls and continuous aligned steel filamenls. Appreciable impvocetnents in fatigue strength were obseved in all syslems inzvesLigated, the degree of sl renglhenng-increasing with increasing volume fraclion of reinforcement. The mode of fatigue failure was found to be a function of colutrre jp-actiotz and was also noted to be controlled by the relative fatigue and strength characlerislics of the matrix and reinforcemenl. THE advantages to be gained by suitably incorporating high-strength filaments or whiskers into metallic matrices are well-recognized.&apos; To date emphasis has been placed on the experimental determination of tensile strengths and elastic moduli of metal matrix composites measured parallel to unidirectionally aligned filaments. Several attempts have been made to relate experimentally measured tensile properties to theoretical values calculated from the properties of the components on the basis of the relatively simple "rule of mixtures" analysis. However, relatively few data have been reported in the literature on the fatigue behavior and mechanism of fatigue failure of metal matrix composites. In a study of fatigue crack propagation in aluminum plus steel wires and aluminum plus tungsten wires, Forsyth et a1.2 found that the incorporation of small numbers of filaments suitably dispersed were capable of substantially reducing the rate of fatigue crack propagation. For this purpose, the strength of the filaments appeared to be more important than the aspect ratio and the authors reported that parallel filaments were not the most favorable orientation for increased strength. In a basic study of the fiber reinforcement of metals, Williams and 0&apos;brien3 report preliminary results which indicate a considerable improvement in fatigue strength in reversed bending fatigue of a steel wire-reinforced aluminum alloy composite. In a study of the influence of interfacial bonding on fatigue behavior, Baker4 has also reported improved fatigue properties in stainless steel-reinforced aluminum composites. In contrast, Ham and place5 report that, although tensile properties are improved greatly by filament reinforcement, the reinforcement of copper with continuous, brittle tungsten wires up to 23 vol pct was comparatively ineffective against fatigue. The authors attribute the poor fatigue properties of the composite to fatigue hardening of the matrix at the tips of cracks which can build up stress concentrations sufficiently large to fracture proximate filaments. Baker and cratchley6 failed to find marked improvements in the reversed-bending fatigue properties of silica-reinforced aluminum. The study was complicated by the complex behavior in a composite during the compres-sive half-cycles imposed in this type of loading. This was manifested in the failure of the composites by de-lamination, a contributing factor being the presence of aluminum oxide at the matrix-filament interface. Prior to the general acceptance of filament-rein-

Jan 1, 1968

By M. E. Shank, J. Wulff

At the present time, the designer of dies for metal powder pressing is handicapped by relative ignorance of stress distribution and frictional effects at the interior surface of the die. Unckell was the first to develop a method for the study of wall friction. He used three Brinell balls on which the die rested during pressing. The total frictional wall force was determined by the size of impression these balls left on a soft metal plate. Since the method does not give radial pressures, or distribution of such pressures, coefficients of friction could not be determined. Although Unckel measured density distribution, he was not able to determine radial or shear stresses. Shaler2 has proposed theoretical expressions for the stress and density distribution within cylindrical compacts during pressing, in accordance with the experimental results of Kamm, Steinberg, and Wulff.3 By application of Siebel&apos;s method,4 Kamm et a13 plotted stress trajectories for two compacts. From the stress trajectories they calculated coefficients of friction from point to point along the die wall. As pointed out by Shaler in the discussion of Ref. 3, these values are based on progressive point-to-point calculations on finite size grid squares across the compact. In the region of the die wall such calculated values may therefore have considerable cumulative error. The purpose of the present paper is to develop an experimental method by which the nonhydrostatic pressures and shears acting on the interior wall of a cylindrical die can be measured. Such measurements can then he correlated with existing data to aid in the explanation of the pressing process. The method used is based on the elastic: properties of the thick-walled tube used as the die. The principle of super-position of force systems on an elastic body is assumed to hold. Electric strain gauges were mounted in adjacent positions on the exterior die wall in order to get an exact measurement of the variation of tangential strain over the length of the die during pressing. While in this paper, measurements in terms of only tangential strains are considered, it is well to note that similar calculations may be set up for axial strains. The latter are not preferred, since they tend to be smaller than the tangential strains and therefore permit less sensitive measurements. Discussion in this work is restricted to compacts pressed from both ends, since the elastic deformation of the die is then more amenable to analysis. Before choosing the electric strain gauge method, a more direct line of attack was considered and discarded. The discarded idea was the insertion of a pressure gauge through a hole in the die wall.* The gauge would have been in the form of a small piston. If pressure were exerted against such a gauge, it would move outward along a radius of the die. One disadvantage of the scheme is its inability to measure shears along the die wall. Another more serious disadvantage is the disturbance caused by the device itself. It would serve to change the forces it was designed to measure. No matter how small the movement of the gauge, when pressure is applied a discontinuity would exist in the wall surface at that point. Due to the stress concentration caused by the hole, abnormal deflections of the die wall would occur around the gauge. During pressing, powder would be forced into the resulting depression. The depression would then become larger with increasing compacting pressure. Powder, not being a fluid, is capable of supporting shear. The ease with which it would flow into the die wall depression to further move the piston is an indication, not of the radial pressure at that point, but of the state of shear retarding the movement. Thus the "pressure" gauge is really a criterion of flowability, and of the capability of the powder to support shear. For these reasons, it was decided that the electric strain method, herein employed, was more reliable, if more indirect. The gauges and lead wires, mounted on the external die wall do not in any way affect the behavior of the metal powder or the die during pressing. Theory of the Method THE EFFECT OF RADIAL PRESSURE ON THE DIE WALL Effect of a Single Small Band of Hydrostatic Pressure Consider a die which is a thick-walled cylinder of outer radius R. and inner radius Ri. If over a small finite length L there is a normal pressure P, a tangential strain distribution at the outer wall results. This is shown schematically in Fig 1. The exact shape of the curve may he predicted by an extension of the theory of a semi-infinite beam on an elastic foundation.6 This

Jan 1, 1950

By Milton E. Wadsworth, J. Brent Hiskey

INTRODUCTION Fifteen years ago a distinguished electrochemist referred to electrochemistry as an "underdeveloped science " In the article in question, Professor Bockris (1) stated that many areas of.natura1 phenomena and applied technology are not perceived as being electrochemically based At that time, this was especially true for much of non-ferrous extractive metallurgy and was a particularly accurate description of hydrometallurgy During the last decade, there has been considerable advancement in applying the theory of electrochemistry to our know1 edge of hydrometallurgical processes and in understanding the mechanisms of underlying electrode reactions. Impressive as these advances are, there is still a growing need for electrochemical research of mineral systems and electrochemical engineering to apply this work in practical situations In a broad sense electrochemistry is defined as the physical chemistry of ions in solution and of phenomena which occur at the electrified interface. Bockris and Reddy (2) refer to electrochemistry as being divided into two fundamental domains, ionics and electrodics ionics is restricted to the behavior of ions in solutions, examples being many familiar redox processes Electrodics represents the main part of electrochemistry, and is the study of charged interfaces and the conditions governing charge transfer reactions across them. Considering hydrometallurgical applications, electrodics suggests the following relationship for a conducting solid (bulk or surface)

Jan 1, 1981