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By C. L. Warwick, A. B. Parsons

The papers and discussion appearing in this volume were presented at a symposium jointly sponsored by the American Society for Testing Materials and the American Institute of Mining and Metallurgical Engineers and held at Philadelphia, Pa., November 29, 30, and December 1, 1944. Late in January, 1944, Lieut. Col. C. H. Greenall, Officer-in-Charge of the Laboratory Division, Frankford Arsenal, Ordnance Department, U.S.A., suggested to the American Society for Testing Materials that it might be a propitious time to arrange for a symposium on stress-corrosion cracking at the Annual Meeting of the Society in June, and agreed to make available a number of papers relating to work being carried out at that Arsenal. The Society's Committee B-5 on Copper and Copper Alloys, Cast and Wrought expressed keen interest in the symposium, and other Society committees were contacted and agreed to cooperate. Since the subject is one of primary interest also to the American Institute of Mining and Metallurgical Engineers, it was arranged that the two organizations would jointly sponsor the symposium. A Symposium Committee was formed under the joint leadership, for A.S.T.M., of Carter S. Cole, then Chief of the Metals Branch, Conservation Division, War Production Board and now Engineer on the Headquarters Staff of the Society; and, for A.I.M.E., of E. A. Anderson, Chief of Metals Section, Research Division, New Jersey Zinc Co. (of Pa.) and chairman of the Program Committee of the Institute of Metals Division. The Symposium Committee was constituted as follows:

Jan 1, 1945

By Joseph Pogue

THE, prices of crude petroleum and its derivatives have shown an upward trend from 1915 to 1920, and a downward trend from 1920 to 1923, see Table 1. Over the former period, oil prices were dominated by the rapidly increasing demands and inflation incident to the war and its aftermath, while over the latter period oil prices were influenced at the outset by deflation and then by the conditions of overproduction that have characterized the past three years. The purpose of this paper is to analyze the broader features of the more recent price movements in the petroleum industry and to relate these features to basic economic conditions in the industry. INDEX NUMBERS OF OIL PRICES The analysis and comparison of price movements may be facilitated by converting actual prices into relative prices, or index numbers, with 1913 taken as a base of 100. In this way, the various price groups are expressed as percentages of the 1913 prices and may thus be readily compared with one another or with the average prices of other commodities similarly expressed. Table 1 gives the index numbers representing the average prices of crude petroleum, gasoline, kerosene, fuel oil, lubricating oils, and all commodities. The last named is the index of all commodities as published by the U. S. Bureau of Labor Statistics and .is widely accepted .as the official measure of the general price level. The index numbers of oil prices were calculated by the writer from weekly quotations published in trade journals.

Jan 3, 1924

By G. E. Perry, R. D. Seba

The steam soak process is the most widely applied and most successful thermal supplemental recovery process in use today. This process, which consists of injection of steam in various quantities into a well that is subsequently used as a producer, can be repeatedly applied to the same well. The treatment, if successful, will increase the production rate of the well for a given period. For this reason, the steam soak process should be considered primarily as an acceleration method rather than as a method for producing oil that could not be recovered by primary means. However, application of this process to reservoirs containing viscous crude may produce oil that otherwise would have zero present value or would be produced at such low rates by primary methods that it would not be profitable. A major necessity for the successful application of the steam soak process is a source of natural energy. This source of energy may exist in one or more of the following forms: expansion of fluids, compaction, gravity drainage. This study was undertaken to determine the effect of gravity drainage on steam soak production and recovery and to develop a method for predicting production rates, ultimate recovery, and heat requirements when applying this process to a reservoir in which the primary driving mechanism is gravity drainage. (For additional discussion of some of the factors that affect recovery of viscous oils by the steam soak process, see Ref. 5.) Model The model developed for analyzing the performance of the steam soak process in gravity drainage reservoirs is a modified form of that developed by Matthews and Lefkovits.1,2 The model used in this study consists of two concentric cylindrical volumes of productive formation with cap and base rock of impermeable material. The inner cylinder, extending from the radius of the wellbore to some predetermined radius, is referred to as the hot zone; and the outer cylinder extending from the exterior boundary of the hot zone to the outer drainage boundary will be referred to as the partially heated zone. Fig. 1 is a schematic cross-section of the model, indicating its thermal properties. Horizontally the reservoir is divided into two regions, the upper region having a high gas saturation and residual liquid saturation, and the lower region containing a high liquid saturation. The boundary between these two regions is referred to as the free surface, which drops and changes shape as fluid is produced from the reservoir. The model was used to analyze the steam soak process by applying the following assumptions: 1. The horizontal formation is composed of one or more homogeneous noninterconnected layers containing incompressible fluids. Each layer is treated separately. 2. The hot zone is heated by the initial soak and is maintained at the steam temperature corresponding to atmospheric pressure by resoaking. 3. The height of the free surface at the producing well is at all times zero (producing well is pumped off). 4. The position of the free surface at the start of

Jan 1, 1970

By Norman F. Schulz

The technical excellence of separation achieved in a mineral concentration process, or any other process where two constituents of any kind are physically separated from each other, is expressed uniquely and quantitatively by the separation efficiency (E,): E. = (R - R,), where R is the percentage of the valuable constituent and R, the percentage of the waste appearing in the concentrate. The separation efficiency meets all the usual requirements of a true efficiency and is independent of the nature of the process used. It can be visualized as the percentage of the feed material that, in effect, actually undergoes complete separation while the rest of the feed is distributed randomly and unchanged into the two separation products. The problem of quantitatively assessing the results of a mineral concentration process recurs whenever one tries to decide which of two similar test results is more desirable. Although economic factors may greatly influence the eventual choice of process, they usually have very little to do with the technical excellence of a separation and are, therefore, not a consideration at this point. Concentrate grade and recovery, used simultaneously are the most widely accepted measures of performance, and if both the grade and the recovery are greater for one case than for another, the choice is simple. However, when the results of closely competitive operations are compared, it often occurs that one set of test results shows a higher grade and a lower recovery than another and the choice is no longer obvious. Laboratory investigations of a mineral concentration process applied to a given feed material can often be designed to yield successive paired values of concentrate grade and recovery over the practical range of the course of a separation process.' These results may be plotted as some combination of the cumulative values of grade, weight recovery, or unit recovery in the concentrate. The resulting correlations for two slightly different sets of conditions can then be compared qualitatively, or even quantitatively in particular cases.2 Such comparisons are not applicable, however, to individual concentration test results. The reduction of a separation test result to a single efficiency figure, preferably as a percentage of ideality, would afford the simplest and most precise means for comparing the results of competitive tests. The effective proportion of feed material that undergoes complete separation in any real concentration process, hereafter referred to as "separation efficiency," is such a figure. It is essily calculated from the usual feed and product data and can even be evaluated, in many cases, from data in publications describing various concentration processes. Mineral Concentration Processes and Their Evaluation Mineral Concentration Processes: The overall concentration process may be subdivided into a liberation process which severs the bonds between unlike mineral species, and a separation process, which sorts the resulting liberated particles into two products—a concentrate rich in mineral A and a tailing lean in mineral A. A perfect mineral concentration process is represented by the idealized scheme shown in Fig. 1 in which liberation and separation are not differentiated. The feed mixture consists of two mineral types which are completely liberated early in the process and then sorted by type. All the mineral particles of type A which respond uniquely to the selection forces acting in the ideal separator, report to the concentrate, while all the mineral particles of type non-A report to the tail-

Jan 1, 1971

By Ogden Malin

IN conducting the manufacture of extruded brass rods and brass forgings it has been noticed that there is considerable variation in the physical properties, particularly the machinability of different rods and forgings, even though the composition, working temperatures and method of manufacture remain the same. It is the purpose of this paper to attempt to establish the cause and extent of this variation, and also to determine whether variations in composition within certain defined limits influence hardness and machinability to any marked degree. The writer believes that this variation probably is due to the variation in grain size of the metal, therefore the microstructure of several compositions under various conditions of working were examined in an effort to establish this as a fact.

Jan 1, 1932

By Thomas C. Wilder

Jan 1, 1965

By M. C. Udy, F. W. Boulger

AN incomplete phase diagram for the U-Ti systern was determined earlier 1 and more recently, a tentative diagram was presented for the uranium-rich end of the system.' In the present re-examination of the whole system of U-Ti alloys, high purity materials were used. Melting stock for the alloys was high purity uranium, containing about 0.09 pct C as the only appreciable impurity, and high purity iodide-process titanium purchased from New Jersey Zinc Co. Both metals were cold rolled to about 1/6 in. thickness, sheared to about I/' in. squares, and cleaned by pickling. The alloys were arc melted under a helium atmosphere in a water-cooled copper crucible. A thoriated-tungsten electrode was used. The furnace chamber was evacuated, then flushed with helium, prior to each melting. It was finally filled with stagnant helium at one atmosphere pressure. Each alloy was remelted three times after the original melting, to insure homogeneity. The alloy button was turned bottom side up before each re-melting operation. Some 22 alloys were examined. Their compositions were spaced at appropriate intervals between 100 pct Ti and 100 pct U. Analyses were made on chips taken after fabrication. The major contaminant was carbon, which varied from 0.03 to 0.08 pct. It appeared in the microstructure as titanium carbide. Alloy compositions were calculated to a carbon-free basis for consideration on the diagram. Tungsten and copper, possible contaminants from the melting operation, were generally less than 100 parts per million each. Fabrication All alloys were forged and rolled to bars approximately V8 in. square. They were clad either in SAE 1020 steel or in a 5 pct Cr-3 pct Al-Ti-base alloy, depending on the fabrication temperature. A temperature of 1800°F (980°C) was used for alloys near the compound composition. This necessitated using the titanium-base alloy, since iron reacts with titanium at this temperature, producing a low melting alloy. Other alloys were fabricated at 1450°F (790°C), using steel jackets. No iron-titanium reaction occurred at this temperature. The jackets were welded in place in an argon atmosphere. Those alloys sheathed in steel were declad and then reclad between rolling and forging operations. On the other hand, those clad with the titanium alloy were cut to a roughly rectangular shape prior to clading and were then carried through both the forging and rolling operations without opening. Those alloys near the compound composition were found to be cracked when the clading was removed. The cracked materials had been plastically deformed, however, and at least some of the cracking had OCcurred during cooling. Heat Treatment The rolled bars, after being declad and shaped to remove surface contamination, were all given an homogenizing treatment of 160 hr at 2000°F. (Samples were taken for analysis following the declading and shaping operations.) All were heat treated at the same time in one furnace, but each was sealed in a purified argon atmosphere in an individual Vycor glass tube. Argon pressure was such that it was approximately atmospheric at temperature. One end of each tube contained titanium chips and this end was heated to 1200°F (650°C) for 10 min prior to the heat treatment. This purged the atmosphere of residual reactive gases. The balance of the tube was warmed during the purge to liberate adsorbed moisture and gases, which also reacted with the hot chips. The bars were furnace cooled from the homogenization treatment. Specimens of each alloy were water quenched after 2 hr heating at 1000°, 1200°, 1400°, 1600°, 1800°, and 2000°F (540°, 650°, 760°, 870°, 980°, and 1095°C). In addition, some were treated at intermediate temperatures of 1300°, 1500°, and 1700°F (705", 815", and 925°C) and at 2150°F (1175°C). Specimens, about '/s in. cubes, were cut from the bars, sealed in individual Vycor tubes, and heat treated as described. All specimens heat treated at the same temperature were processed together. Samples were quenched by breaking the Vycor tube rapidly under water. Metallographic Examination Specimens were mounted in bakelite and ground wet on 180 grit paper held on a 1750 rpm disk. They were then ground wet by hand, using 240, 400, and 600 grit papers. The rough grinding was continued long enough to get well below the surface. Specimens were mounted separately because of the variation in the rate of etching between alloys. The specimens were polished with rouge on a 4 in., 1725 rpm wheel covered with Miracloth. Alloys on the titanium side of the compound composition were etched with a solution of 2 pct hydrofluoric acid in water saturated with oxalic acid. A few crystals of ferric nitrate were added as a bright -ener. Specimens were immersed 5 sec, polished to remove the etch, then re-etched. With the higher titanium alloys, it was often necessary to start the etch on the polishing wheel, because of the formation of a passive film. In some instances, a plain 2 pct hydrofluoric etch was satisfactory. For the alloys on the uranium side of the compound, a distinction between the compound and the uranium phase developed after standing a short time in air. This could be hastened by the application of heat, such as obtained by placing the specimen on a radiator. A deep etch was necessary to develop details in the uranium-rich phase, such as the Widmanstaetten pattern sometimes obtained by quenching y uranium. A 2 pct hydrofluoric acid solution was used for this deep etching.

Jan 1, 1955

By V. Koump, T. F. Perzak, R. H. Tien

A series of experiments were carried out in which the rates of propagation of the liquidus and the eutectic fronts Mere measured during essentially one-dimensional freezing of Al-Cu alloys. The dimensions of the ingots were 3 by 5 by 6 in. Three different alloys containing 0.1, 4.5, and 17 pct Cu were used in these experitments. For each alloy the rate of heat removal was varied to give a total jreezing time in the range 3 to 30 min. The results of these measurements cowlpared favorably with the theoretical model of freezing of binary alloys with time-dependent surface temperature. IN engineering analysis of solidification of commercia1 steels and nonferrous alloys it is a common practice to assume that an alloy freezes by propagation of an isothermal solidification front, i.e., essentially as a pure metal. In two recent theoretical investigations'j2 the present authors explored the possibility of a more realistic approach to the problem of solidification of alloys. In the proposed model the freezing of an alloy is assumed to take place by propagation of two isothermal fronts, i.e., the liquidus front and the solidus (or eutectic) front. The region between the two fronts contains both liquid and solid and is referred to as the solid-liquid region. The width and the solid content of the solid-liquid region vary with alloy type, solute concentration, and cooling rate. For a given alloy system, initial concentration of solute, and the mode of heat removal, the proposed model yields the temperature distribution within the solid skin, temperature, solid fraction, and concentration distributions with the solid-liquid region, and the rates of propagation of the liquidus and the solidus fronts. This model is obviously of considerable practical importance in engineering analysis of solidification processes, since it gives a more realistic estimate of skin strength during solidification and a better estimate of the total freezing time. Before the new model can be used with confidence, however, it is necessary to test this model experimentally. The experimental testing of the proposed model is a relatively simple matter since the effects to be measured are large and a relatively simple experiment will suffice. The theoretical model predicts, for example, that during freezing of an alloy containing substitutional type solute (negligible diffusion in the solid during freezing) the solid-liquid region occupies an appreciable portion of the ingot, even at low concentration of solute.' Another prediction of the theo- V. KOUMP, formerly with U. S. Steel Corp., is now with Research and Development Center, Systems and Process Division, Westinghouse Electric Corp., Pittsburgh, Pa. R. H. TlEN is Senior Scientist, Fundamental Research Laboratory, U. S. Steel Corp., Research Center, Monroe ville, Pa. T. F. PERZAK, formerly with U.S. Steel Corp., is now with Fiber Industries, Greenville, S. C. Manuscript submitted March 6, 1968. IMD retical model, easily verifiable by experiment, is that the rate of propagation of the solidus (or eutectic) front increases as the solidus front approaches the center of the slab. This prediction is contrary to well-known behavior of the solidification front during freezing of pure metals, where the rate of propagation of the solidification front decreases with time and freezing is completed at the lowest rate. A rather severe test of the proposed model is provided by comparison of theoretical predictions and experimental measurements of the effects of cooling rate and composition on the rates of propagation of the liquidus and the eutectic fronts. In order to test the soundness of the formulation and the method of solution of the problem of solidification of alloys a series of experiments were carried out in which the rates of propagation of the liquidus and the eutectic fronts were measured during essentially one-dimensional solidification of A1-Cu alloys. The A1-Cu system was chosen strictly as a matter of convenience. Three different alloys containing 0.1, 4.5, and 17 pct Cu were used in these experiments. For each alloy the rate of heat removal was varied to give the total freezing time in the range 3 to 30 min. The results of these measurements are compared with the predictions of the theoretical model of solidification of binary alloys, with time-dependent surface temperature.' Before the experiments described in this paper were undertaken, a serious attempt was made to utilize the measurements of previous investigators to test the theoretical model. In the course of this preliminary study a careful review was made of experiments of Pellini and coworkers3 and Doherty and Melf~rd.~ The measurements in Pellini's work were carried out using a steel containing at least four major components. Evaluation of the solid fraction-temperature relation for this steel (required in the theoretical model) is difficult and uncertain. Doherty and Melford, on the other hand, measured the solid fraction-temperature relation experimentally, but did not give sufficient data to explore the effects of composition and the cooling rates on solidification. Hence it was not possible to utilize these measurements to test our theoretical model. EXPERIMENTAL METHOD The experimental technique used in this investigation differs somewhat from the more conventional techniques employed in solidification studies. This technique was developed primarily to eliminate con-vective mixing in the molten metal caused by pouring of molten metal into the mold. In our experiments A1-Cu alloys were melted directly in the mold. The mold assembly used in solidification experiments is shown in Fig. 1. The mold was fabricated from *-in. stainless-steel sheet. The dimensions of

Jan 1, 1969

By S. Ramachandran, R. G. Woolery

INTRODUCTION Union Carbide is currently operating an in-situ leach project on the Palangana Dome area in Duval county. This deposit meets all the requirements for in-situ leach in that the ore (1) is below the water table, (2) is in a permeable horizon, (3) is amenable to chemical leaching, and (4) is confined by impervious layers. This project has been under commercial production since 1976, and its capacity has been expanded on three occasions since going on-stream. Recently, additional uranium reserves were discovered on the Rogers-Cardenas (R-C) property about 32 km north of the Palangana operation. The ore is located within the Oakville sands and its characteristics are quite similar to those of the ore at Palangana. Both are an unconsolidated Arkosic sand high in clay and calcium carbonate. The R-C ore, however, is somewhat coarser with a mean particle size of 0.15 mm as compared to a mean particle size of 0.07 mm for the Palangana ore. In all respects it would appear that this ore would be a candidate for in-situ leach as a satellite operation to Palangana. Unfortunately, R-C ore is above the water table and, therefore, not amenable to the Palangana practice. Because of the limited known reserves in this deposit, it is readily apparent that conventional mining and milling are out of the question. However, because of its proximity to our Palangana operation, it seemed worthwhile to consider other options. The most viable route based on our past experience was to heap leach the ore. Our recent success at our Gas Hills facility and our Maybell operation, in employing a heap leach practice to our marginal reserves seemed to be a logical approach for processing this ore. Our experiences at both locations are described in "Heap Leaching - A Case History" by R. G. Woolery et al., Mining Engineering, March 1978. In both instances the process is an acid leach circuit and acid consumption averages 20 kg/t H2SO4. A preliminary feasibility study showed that because of the high strip ratio required for the R-C project to be successful, additional ore reserves must be located and that a method of heap leaching with an alkaline circuit would have to be developed. As a result of this paper study, the decision was made to proceed with a program of additional exploration drilling to determine the total ore reserves that could be mined economically. The Mining Department will evaluate each ore zone for cutoff grade, strip ratio, and expected mining cost. At the same time, a laboratory program to evaluate the available core samples for amenability to heap leaching with respect to an estimate of uranium recovery and processing costs was developed. This program is currently in progress, and at this time, we are just completing our process amenability study. BENCH-SCALE EVALUATION OF THE R-C ORE The initial bench-scale slurry leach tests on the R-C ore showed an acid consumption in excess of 200 kg/t H2SO4. These data, of course, discouraged us from considering this process route. Not only would the acid cost be prohibitive, but the gypsum generated by the reaction of the sulfuric acid with the calcium carbonate of the ore would severely effect the percolation of the lixivant. For this reason, the laboratory program was directed toward an alkaline circuit compatible with heap leaching. Because of the proximity of the R-C property to our Palangana operation, it seemed advisable to integrate the processing of this ore into the production at Palangana. Doing so would enable us to bring the R-C property into production by merely enlarging our present facilities at Palangana; otherwise, construction of a grass roots plant would be necessary. Ideally, the simplest method would be to construct the heaps at Palangana and employ an ammonium carbonate/bicarbonate leachant compatible with the in-situ production liquor. The product liquors could then be co-mingled or processed separately as desired. To determine if this goal was practical, samples of the R-C ore were obtained, and a laboratory program initiated. Heap leach amenability testing consisted of preliminary bench-scale evaluation to determine optimum solution strength and ultimate uranium recovery, followed by small column tests to confirm the bench-scale metallurgy and to determine percolation characteristics. These bench-scale tests are being followed by pilot-scale testing approximating field conditions. As expected, the bench-scale tests showed that the dissolution rate is considerably slower for alkaline leach than has been our experience in acid leaching. Because of the slower reaction rates, product liquor grades will be lower than for acid, as greater volumes of solution are required for satisfactory uranium extractions. The greatest influence on reaction times found in the laboratory was the carbonate/bicarbonate strength and oxidant addition. However, the higher salt concentration reduced the efficiency of the IX resin circuit and about 25g/L salt proved to an upper limit compatible with subsequent IX treatment. The oxidant contributed significantly to the early extraction rate but seemed to have only minimal effect on the total practical U308 extracted or the time required to achieve it. This variable will require larger scale testing to determine if the added cost of the oxidant is actually justifiable. Thus, the small-scale laboratory slurry tests, based on the 0.088% U308 sample available, indicate that leaching at 25g/L ammonium carbonate/bicarbonate, with or without oxidant, we might expect an 80-85% U308 extraction on this ore.

Jan 1, 1979

By L. D. Keller

The application of hydraulic concentration to large scale operations has been effectively accomplished by the use of the SiphonSizer. Operation has been simple, automatic and essentially trouble free. The use of the primary desliming SiphonSizer on magnetic taconites has shown an improvement in grade of concentrate and an increase in recovery over conventional hydroseparators. Magnetic concentrates have been further deslimed and upgraded in SiphonSizers by floating a coarse middling product away from the heavier concentrate. The application of the Siphon-sizer to closed circuit grinding has met with only partial success to date. Hydraulic concentration of minerals has been practiced for a good many years. Until recently, however, the practice has been limited to equipment using a multiplicity of small pockets and relatively low tonnages and flows. The adaptation of the SiphonSizer to the concentration and classification of magnetite has changed this concept. Some fifty commercial units varying in size from a 16-ft diam circular unit to a 25x100-ft rectangular unit are currently in operation on magnetic taconites. Additional units up to 38 ft diam are under construction. Depending upon the application in the flowsheet, upgrading varies from 0.75% to 14% Fe in a single stage. To those not familiar with taconite processing, the importance of the struggle to remove economically as much silica as possible may not be fully appreciated. Perhaps some figures pertaining to transportation costs will underscore this important process. If the silica content of the concentrate from a 10,000,000 ton per year plant could be reduced by I%, a savings in boat freight, at $2.00 per ton, would amount to $200,000 annually! THE SlPHONSlZER The SiphonSizer, as illustrated in Figs. lA, 1B and 2, is a hydraulic classifier in which the hydraulic water is distributed uniformly across the bottom of the vessel by means of a system of headers (1 and 2), jet pipes (3), and nozzles (4). The depth of the teeter bed is automatically maintained by the siphon-float assembly. The feed is introduced through a feed well (5) and separated into two fractions by the effects of rising water and the density of the teetered bed. The magnetite fraction is discharged by the siphon (12) while the fine slime and light middling overflow a peripheral weir (9) to the overflow launder (6). The bed depth is controlled automatically by float valves (7), which are responsive to changes in the height of clear water supported in the superelevation tubes (8) by the density of the teetered bed. On top of the float (7) is a needle valve (10) which permits

Jan 1, 1963

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By Charles S. Barrett

This paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstruc-tures. About 1200 exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,' and a number of these have been selected to illustrate the results obtained. prints are also included showing the common types of falsities—to borrow a term from the biological field, the "artifacts." ln brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. In addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains, since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. Specimen Preparation and Photographs Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for these polishing and etching (each successive polish becoming less severe and each etch lighter), since the fina1 etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and 16, the replicas used were of silica, deposited upon polystyrene and floated from the polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1944

By Charles S. Barrett

THIS paper is a progress report covering metallographic applications of the electron microscope that have been made during the past year at Carnegie Institute of Technology. An account is presented of the techniques that have been most satisfactory, the difficulties encountered, the resolution obtained, and the peculiarities that have been noted in the microstructures. About 12m exposures have been made during the year on the instrument, which is an RCA type B2 transmission microscope,1 and a number of these have been selected to illustrate the results obtained. Prints are also included showing the common types of falsities-to borrow a term from the biological field, the "artifacts." In brief, the paper is a record of our attempt to determine the value of the electron microscope in the study of the structure of metals and alloys. n addition to comments on techniques and the quality of photomicrographs obtainable with them, the paper discusses the nature of the etch attack on a few metals, and the possible relation between the fine structure revealed by etching and the mosaic block structure of the grains. Since numerous papers and reviews are available on the subject of imperfection in crystals, the comments here may be very brief; in fact, are restricted almost entirely to points having to do with recent theories relating the strength of metals to imperfections and to spacings of slip lines. SPECIMEN PREPARATION AND PHOTOGRAPHS Mechanical polishing by hand was used throughout this work. Precautions that must be taken in microscopy at high magnification, which have been well explained by Vilella in his book on Metallographic Technique for Steel, are likewise important with the electron microscope. This applies particularly to the need for repeated polishing and etching (each successive polish becoming less severe and each etch lighter), since the final etch should in general be no heavier than is used for oil-immersion optical microscopy and in many instances should be much lighter (compare Figs. 6a and 7a, 6d and 7b). An extremely light etch, of course, is incapable of cutting through a flowed layer of appreciable thickness. Unquestionably it would be very advantageous in each instance to compare the structures obtained by electrolytic polishing with those obtained by mechanical polishing, but difficulties with the electrolytic method have prevented this in the following collection of prints. The choice of etchant is important, of course; for example, picral proved superior to nital for tempered martensite. With the exception of Figs. Ib and IC, the replicas used were of silica, deposited up0n polystyrene and floated from the polystyrene in ethyl bromide according to polystyrene in ethyl bromide according to the method of Heidenreich and Peck.2 The samples were mounted in Bakelite, polished and etched, then the polished Bakelite

Jan 1, 1943

By T. Federighi, S. Ceresara, C. Panseri

The results of an exploratory investigation by means of resistivity measurements at -195ºC, on the aging characteristics of a set of Al-Mg alloys with a maximum content of 7 pct Mg, are reported. Whereas for dilute alloys (Mg < 1.5 pct) only a decrease in resistivity is observed at about 100°C (due to the elimination of quenched-in vacancies), for more concentrated alloys such a decrease is preceded by an increase in resistivity in the range between -60ºand +40°C. Following some previous suggestions, this increase is considered as good evidence for clustering of solute atoms @reprecipi-tation process). From the analysis of the results it appears that, although the process is substantially similar to that observed in other Al-rich alloys, it is characterized by a strong interaction between vacancies and zones. THE process of formation of Guinier-Preston zones, i.e., preprecipitation,1&apos;2 which occurs during the aging at about room temperature in many supersaturated aluminum-rich alloys, has been extensively investigated in the past few years by several workers.2,3 owever, a very interesting question arises when the case of Al-Mg alloys is considered: although it is very easy to supersaturate Al-Mg alloys, just in the same way as for many other aluminum alloys showing preprecipitation, only very little experimental evidence was available until a short time ago in the literature supporting the existence of "natural" aging in supersaturated Al-Mg alloys (see, for example, Refs. 4 to 6). On the other hand, as is well known, the X-ray method is not useful in this case because the X-ray scattering factors of magnesium and aluminum atoms are about the same. Recently, however, Cordier and Detert7 have stressed that during the aging at about room temperature of a supersaturated Al-Mg 10 pct alloy it is possible to detect an increase in resistivity; since, as is well known, such an increase is observed also in most alloys showing preprecipitation, the above authors have interpreted their results as evidence for the formation of magnesium-rich clusters (or Guinier-Preston zones) during the aging. In the course of or ientative investigations on preprecipitation in several aluminum-rich alloys, we also could detect a similar phenomenon in more dilute Al-Mg alloys, see Instituto Sperimentale Metalli Leggeri, Annual Report, 1959, and also Ref. 8. Since the details of our observations, although of a preliminary nature, differ from those of Cordier and Detert and allow one to draw a more advanced picture of the preprecipitation process in Al-Mg alloys, we have thought it useful to report our results in this paper and to comment on them briefly.

Jan 1, 1963

By G. Sachs, G. Espey

It is well known that high residual stresses are created in tubing by the sinking process, in which no internal tool or mandrel is used.l-4 In this process, the wall thickness is usually slightly increased.4,5 In tube drawing with a plug, the residual stresses are gradually reduced with increasing reduction of wall, and, by the conventional approximation methods of stress measurement, no stress is detected in tubing in which the wall reduction is over 50 per cent of the total reduction in cross-sectional area.l,6 It has also been observed that higher stresses are set up by the use of wide-angle dies than by acute dies.? &apos;he actual stress distribution in drawn tubing has been investigated by a few workers,7"9 but has not been related to the conditions of the drawing process. Some attempts have been made to correlate accelerated cracking tests for stresses in brass products with the magnitude of the circumferential stresses and the condition of the metal. l-10 Materials and Preparation The material used in this experiment was commercial cartridge-brass (70 per cent Cu, 30 per cent Zn) tubing in the straightened and annealed condition.† This tubing was of various outside diameters and had a wall thickness of 0.032 in. It was sunk to 1/2-in. outside diameter by means of an experimental 10,000-lb. hydraulic draw-bench, with a maximum drawing speed of 8 ft. per minute. All dies were of 1/2-in. diameter. Various die materials and contours were used in order to study the effect of die design on residual stresses in the tubing; the specifications for the dies are given in Fig. I. Castor oil was used throughout as lubricant. Chattering occurred in sinking some of the tubing, particularly when dies having the more acute angles were used, but the tubes showing chatter marks did not differ markedly from those with a smooth surface regarding the magnitude of residual stress. The source of the chattering has not yet been revealed. The wall of the tubing becomes thicker during s nking, as previously observed.4,5 The increases in wall thickness were 3, 7 and 9.5 per cent on the average for 6, 20 and 33 per cent reductions in diameter, no effect of the contour being noticeable. The reductions mentioned throughout this investigation do not consider this fact, but are reductions of the outside diameter. For the evaluation of the residual stress two fundamentally different methods were used. The approximation methodl,ll of splitting a certain length of tubing was employed to obtain a bird&apos;s-eye view of the effect of various drawing conditions on the circumferential stress measured by the diameter change occurring On splitting. For

Jan 1, 1942

By G. Sachs, G. Espey

It is well known that high residual stresses are created in tubing by the sinking process, in which no internal tool or mandrel is used.l-4 In this process, the wall thickness is usually slightly increased.4,5 In tube drawing with a plug, the residual stresses are gradually reduced with increasing reduction of wall, and, by the conventional approximation methods of stress measurement, no stress is detected in tubing in which the wall reduction is over 50 per cent of the total reduction in cross-sectional area.l,6 It has also been observed that higher stresses are set up by the use of wide-angle dies than by acute dies.? &apos;he actual stress distribution in drawn tubing has been investigated by a few workers,7"9 but has not been related to the conditions of the drawing process. Some attempts have been made to correlate accelerated cracking tests for stresses in brass products with the magnitude of the circumferential stresses and the condition of the metal. l-10 Materials and Preparation The material used in this experiment was commercial cartridge-brass (70 per cent Cu, 30 per cent Zn) tubing in the straightened and annealed condition.† This tubing was of various outside diameters and had a wall thickness of 0.032 in. It was sunk to 1/2-in. outside diameter by means of an experimental 10,000-lb. hydraulic draw-bench, with a maximum drawing speed of 8 ft. per minute. All dies were of 1/2-in. diameter. Various die materials and contours were used in order to study the effect of die design on residual stresses in the tubing; the specifications for the dies are given in Fig. I. Castor oil was used throughout as lubricant. Chattering occurred in sinking some of the tubing, particularly when dies having the more acute angles were used, but the tubes showing chatter marks did not differ markedly from those with a smooth surface regarding the magnitude of residual stress. The source of the chattering has not yet been revealed. The wall of the tubing becomes thicker during s nking, as previously observed.4,5 The increases in wall thickness were 3, 7 and 9.5 per cent on the average for 6, 20 and 33 per cent reductions in diameter, no effect of the contour being noticeable. The reductions mentioned throughout this investigation do not consider this fact, but are reductions of the outside diameter. For the evaluation of the residual stress two fundamentally different methods were used. The approximation methodl,ll of splitting a certain length of tubing was employed to obtain a bird&apos;s-eye view of the effect of various drawing conditions on the circumferential stress measured by the diameter change occurring On splitting. For

Jan 1, 1942

By Leslie F. Tedsen, Alan E. Flanigan, John E. Dorn

IT is necessary occasionally to use aluminum-alloy sheet where moderately elevated temperatures are encountered. Considerable attention has been directed toward determining the influence of "artificial aging" on the room-temperature properties of the precipitation-hardenable alloys, as testified by numerous company reports and by references 1 to 4. Investigations on the properties at elevated temperatures are few, however,5-7 and have not always covered the range of times and temperatures of greatest interest. The present investigation was instituted to overcome this deficiency. The work was done for the Office of Production Research and Development of the War Production Board, under the supervision of the War Metallurgy Committee, as a part of the "restricted" Project NRC-548. It has been released for publication by the Office of Production Research and Development. As is well known, the high-strength aluminum alloys achieve their remarkable properties as a result of precipitation-hardening. In production they are subjected to a solution heat-treatment followed by quenching, to retain the supersaturated solid solution. The solution treatment is followed by "aging" (precipitation-hardening) either at room temperature or at a suitable elevated temperature. A considerable increase in tensile and compressive yield stresses results from precipitation at room temperature ("natural aging"). Through the elevated-temperature process ("artificial aging") it is possible to obtain values of yield stress considerably higher than those attainable by natural aging. The increase in yield stress is accompanied by a smaller gain in ultimate tensile stress and by a decrease in elongation. During [TABLE I.-Sources of Materials Used in the Testing Program MATERIAL ORIGIN AND TREATMENT 24S-T Alclad.... From Lockheed stock. 24S-RT Alclad... Direct from mill. 24S-T80 Alclad.. 24S-O Alclad from Lockheed stock, solution-heat-treated (925°F., water quench) and aged at 375°F. for t0 t % hour. 24S-T8I Alclad.. 24S-T Alclad from Lockheed stock, plant stretched up t0 I per cent and aged t0 ± % hr. at 375°F. 24S-T86 Alclad.. 24S-RT Alclad from Lockheed stock aged 534 ± 34 hr. at 375°F. 6IS-W (bare).... From Lockheed stock. 6IS-T (bare) 6IS-W (bare) from Lockheed stock aged 8 hr. at 350°F. XB7SS-T Alclad. From Lockheed stock.] the first stages of artificial aging the yield stress increases steadily until it reaches a maximum value. In this condition the material is said to be "fully aged." Further exposure results in "overaging," attended by a steady decrease in yield stress. In the production of the artificially aged materials, temperatures and times are selected to achieve full aging. The following important characteristics are associated with the process: I. The higher the temperature, the more rapidly is the fully aged condition attained.

Jan 1, 1945

By T. E. Leontis, D. H. Feisel

MAGNESIUM alloys containing rare earth metals have received considerable attention during the past several years because of the need for light alloys having high strength and creep resistance at elevated temperatures. Although much of the work reported earlier has dealt with alloys containing Mischmetal, it has been shown in two previous papersl, V hat distinctly different effects are produced by various rare earth metals and rare earth metal mixtures on the properties of magnesium. For example, much higher strengths are obtained in magnesium alloys containing didym-ium (essentially neodymium plus praseodymium) than in alloys made with Mischmetal, which contains all the rare earth metals in the proportions in which they occur naturally in the monazite ore. Mg-rare earth metal alloys are characterized by a relatively coarse grain size, which greatly impairs castability. The addition of zirconium as a second alloying ingredient has been shown8,7 to refine the grain size, which also produces a distinct improvement in the strength properties. Certain Mg-Mischmetal-Zr and Mg-Mischmetal-Zn-Zr alloy compositions which are currently being produced commercially have been discussed in dytail by Nelson and Strieter,8,4 who also present some in- formation on a Mg-low Ce-Mischmetal-Zr alloy, and by Nelson.8 A patent issued to Jessup, Emley, and Fisher9 emphasizes the superiority of Mg-didymium-Zn-Zr alloys over the corresponding alloys made with Mischmetal. The purpose of this paper is to present the results of an extensive investigation concerned with the effect of increasing amounts of zirconium on magnesium sand casting alloys containing several different rare earth metal mixtures in varying amounts. The effect of the addition of zinc to some of these alloys is also being reported. Preparation and Testing of Alloys The alloys studied in this investigation were prepared in small laboratory melts according to the melting procedures described by Nelson1" as the Crucible Method. Electrolytic magnesium having the composition shown in Table I was used as the starting material. The rare earth metal alloying ingredients used in preparing these alloys were essentially of the compositions listed in Table 11. Some of the didymium-containing alloys were prepared using a Mg-didymium hardener. The rare earth metal content of this hardener analyzed 1.2 pct Ce, 10.4 pct Pr, 80.8 pct Nd, and 7.6 pct La. The zirconium was added in one of three forms: 1) as sponge zirconium obtained from the Bureau of Mines; 2) as a fused salt consisting of 50 pct ZrCl, and 50 pct alkali chlorides from which the zirconium is reduced by the magnesium; or 3) as a Mg-Zr hardener. The alloying procedures and melt hand-

Jan 1, 1958

By J. C. McKinnell

The appraisal of an oil lease may often be mad,? through production decline analysis, which requires description of the functional relationship between the oil production rate and either cumulative production or time. Heretofore, attempts to define the function appropriate to a given set of production data have depended to some extent on subjective procedures. The purpose here is to introduce an objective solution, obtained by combining the principle of least squares with the theory of equations. MATHEMATICAL ANALYSIS The fundamental differential equation appropriate to a general class of decline curves may be written. Solution of Eq. 1 for general boundary conditions may be written in terms of either the cumulative oil production or time: These equations constitute the mathematical expression of the so-called hyperbolic decline. Their complete description for a given set of production data requires the numerical evaluation of the three parameters1.&apos;, n, D, and (go),. For the special case of n = 0, Eq. 2 becomes q. = (q.), - DiN with the corresponding expression in terms of time being q. = (qa),e...........(5) Similarly, for the special case of n = 1, Eq. 3 becomes with the corresponding expression in terms of cumula- tive oil production being q. = (q.),e " &apos;.......(7) Eqs. 4 and 5 constitute the mathematical description of the so-called exponential decline; Eqs. 6 and 7 are the mathematical description of the harmonic decline.&apos;,&apos; Returning to the hyperbolic expressions, Eqs. 2 and 3 may also be written, q: = sNp + b........ (8) and where a = 1 - n; s = (n— 1)D,(q0);"; b = (go):-"; a&apos;=-n;s/= nD,(qo);"; and b&apos; = (go);-. Note that both Eqs. 8 and 9 are linear in either time or cumulative production with respect to an exponential function of the production rate. In other words, a straight line relationship results for both variables when associated with the appropriate power of q,. This fact is of prime importance in the application of statistical analysis. . STATISTICAL ANALYSIS For a given oil lease, the time, production rate and cumulative production are recorded records. To establish predictive formulas from Eqs. 2 and 3, it remains to determine numerical values for the three parameters [n, D, and (q,) .] through an investigation of the past history. Upon interpreting a, s and b as parameters, Eq. 8 may be expressed for every time interval of interest, i, over the past history as follows. (q,): = s(Np), + b........(10) In general, Eq. 10 will not be satisfied exactly, because of the assumptions in the expression of Eq. 1, and the errors and anomalies universally associated with production data. It will instead define the residual, s(Np), + b- CO=d......(11) Squaring both sides and summing over all the data points, m, under consideration yields

By M. R. J. Wyllie, P. F. Southwick

The importance of the so-called "dirty sand" or "conductive solids" problem in electric log interpretation was first stressed in a paper presented in 1949. Since that time the problem has been generally recognized as a most serious one. Several research papers bearing on the theory of the effects of clay contaminants on reservoir rock resistivities have appeared. These papers, while contributing to the theory of the problem, have not offered any practical solution. In the present paper an experimental investigation has been made of the effects of ion-exchange materials on the electrical properties of natural and synthetic porous media. The method used to make synthetic dirty sands is entirely novel and has proved a valuable guide to a better understanding of the properties of dirty sands generally. The effects of ion-exchange materials on both the resistivity and self potential (S.P.) logs have been examined. From the data obtained it has been possible to formulate a simple, practical method whereby electrical logs of dirty sands can be qualitatively interpreted. The method is in all essentials identical to that presently in use for interpreting clean sands. New light has also been thrown on the significance of the term formation factor when it is applied to dirty sands. In 1949 a paper was presented1 which showed that the presence of so-called "conductive solids" introduced considerable complexities into the analysis of the resistivities of dirty sands, i.e., permeable formations containing clay. The reduction of the self potential (S.P.) resulting from the presence of interlaminated shale or interstitial clay in permeable formations has been discussed by Doll.2,3 Noteworthy papers which dilate further upon the effects of shale and clay on the resistivity of permeable formations are those of deWitte,4,5 Berg,6 Wyllie,7 and most recently, Winsauer and McCardell.8 The last authors have endeavored to elucidate the chemistry of the resistivity phenomena in dirty sands in terms of an adsorption hypothesis. Specifically, they attribute the electrolytic conductivity of shales and clays within a permeable formation to an ionic double-layer effect and, for this reason, regard the term "conductive solids" as a misleading one. Some consideration has been given to the effect of dirty sands on the S.P. by Wyllie7 and by McCardell, Winsauer and Williams." Published work to date has cast light only on certain theoretical aspects of the problems created by the presence of clays and shales within permeable formations. One object of this paper is to describe experiments which serve to elucidate further the theory of the dirty sand problem and particularly the significance of the term "formation factor" as applied to dirty

Jan 1, 1955