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Correlation between Metallography and Mechanical Testing By H F MOORE (Henry Marion Howe Memorial Lecture Trans, vol 120 11,000 words ) The lack of effective correlation between metallography and mechanical testing from the days of Reaumur to the present is noted, and two general problems of such cor¬relation are stated (1) the correlation of qualitative test results with quantitative, and (2) the correlation of average results with maximum or minimum results Some correlation has been achieved, notably in the field of heat-treatment and in the study of elastic strength of metals Correlation is in the process of being developed in several other fields, including the quantitative study of the effect of grain size of metal on mechanical properties, of grain size and type of crystalline structure on the sensitivity of metals to weakening at holes, notches and other "stress raisers," and in the study of the starting phases of spreading, "fatigue" cracks Correlation of mechanical test results and metallographic study is needed in the study of such problems as the various theories of failure of metals, the meaning of and tests for service ductility of metals, and the relative damaging effect of defects inherent in metals, such as minute cracks and segregation, as compared with the damaging effect of "imposed" stress raisers, such as screw threads, sharp shoulders, etc The neces¬sity for more correlation of metallography and mechanical testing during student days is emphasized, and also the need of a better understanding on the part of engi¬neers of the significance and limitations of metallographic apparatus and results and of X-ray diffraction This should be matched by a better understanding on the part of metallurgists of the significance and limitations of mechanical tests of metals, of testing machines and strain-measuring apparatus

Jan 1, 1937

By A. S. Yue

It was deemed desirable to obtain an understanding of the vacuum desulfurization process. McKechnie1 has reported that the sulfur content of nickel- and cobalt-base alloys is reduced in vacuo. Keverian and Taylor2 have observed that vacuum melting causes desulfurization of iron-carbon-silicon alloys. Garnyk and samarin3 have desulfurized transformer steel by vacuum treatment. Experiments were conducted in order to investigate the desulfurization of liquid iron under reduced pressures, and to establish the effect of some alloying elements, and various crucible materials. A vacuum-induction furnace of 50-lb capacity was used. The charge was Armco iron. Silicon was added as 90 pct ferrosilicon, carbon as electrode graphite, and aluminum as high-purity aluminum metal. Magnesia and silica crucibles were used, their inside diameters were 5 1/2 and 5 3/8 in., respectively. The temperature was measured with an optical pyrometer and it was held at 1600 1 15°C. Samples were withdrawn with quartz tubes of 6 mm ID, without disturbing the furnace atmosphere. Pressures were measured with an alphatron gage. The experimental results are shown in Fig. 1. They indicate that: 1) Sulfur can be removed from liquid iron alloys by vacuum treatment; 2) The desulfurization is enhanced by the presence of silicon, carbon, and aluminum, all these elements increase the activity of sulfur dissolved in liquid iron;4 3) The pronounced effect of silicon indicates that probably a volatile silicon sulfide is formed, Alcock and Richardson5 have observed a similar phenomenon; 4) The same rate of desulfurization was obtained when the metal was contained in either magnesia or silica crucibles. Dr. J. Keverian has contributed many discussions and recommendations. M. S. Sutliff has helped in conducting the heats. The permission of General Electric Co. for this publication is gratefully acknowledged.

Jan 1, 1960

By Foster Fraas

MOST commercial electrostatic separators utilize the electrical property of conductivity, but although based on the same principles, they are constructed in a variety of forms, a common one being the simple roll type. Some information obtained during an investigation of that type of separator, and which indirectly is applicable to other types, is presented here. NUMERICAL RELATIONSHIP In Fig. I material discharged from hopper 6 is fed onto grounded rotating roll 2. Electrode 3 is at a high electrical potential with respect to roll 2, and any conductive particle in contact with roll 2 therefore acquires an electrical charge of such polarity that, when present in the electrical field, the force on it is in the direction of electrode 3. A detailed description of the charging by conductance as utilized in electrostatic separators may be found in a previous publication.1 As a result of this force, the path of the projected particle is changed in increasing amounts in the direction toward region C as the magnitude of the charge is increased. With the dividing edge 4 the projected particles may be divided into two fractions -those in region C designated as "deflected" or " deflectant " and those in region B designated as "residue." [ ] When material is passed over the roll only once, a complete separation is seldom obtained, therefore most commercial separators contain several roll-separator units in series, and some practical machines use as many as 12. In this paper a "pass" means the passage of material over a single-roll unit. The procedure is to repass either residue B with a low potential on electrode 3 or deflectant C with a high potential on 3. Most electrostatic separations follow a flowsheet of roughing and cleaning either the concentrate or the tailing, on both. In a specific instance, a dry, heated mixture of wet cleaned chromite and garnet from an

Jan 1, 1942

By Frederick Tickell

PETROLEUM engineers are displaying considerable interest in those fundamental properties of matter and energy that control the phenomena of oil and gas production. The subject is a difficult one to investigate by laboratory experiments for two reasons: (1) it is impossible to reproduce in the laboratory the scale of forces and dimensions that exist in the underground reservoir; (2) if we attempt to scale down the dimensions we are unable to reduce all proportionally. It is as if we tried to construct a model blast furnace for the reduction of iron ore, and reduced all lineal dimensions. We should find that the interstices between the miniature chunks of ore would not .permit rapid transfer of gases, that combustion and heat transfer would not take place as in the full size furnace and that, in short, the contraption would not work. Just so, when we attempt to make a reduced scale oil field we find we must have, not only miniature reservoir and miniature wells, but "miniature" sand, oil, gas, etc. Much valuable work, however, has been done along these experimental lines and more will no doubt follow, but investigators should bear this point in mind and strive to attain dimensional homogeneity and dynamical similarity in order that their conclusions may be translated into terms applying to the oil reservoir. As Gibson says,1 "These conditions are attained when all terms of the physical equation have the same dimensions, . . . when all corresponding particles of the two systems trace out similar paths and when the velocities are such as to make all corresponding forces acting on two such particles in the same ratio. It is the purpose of this paper to discuss the mechanics of fluid movement as it pertains to the oil pool and to point out the complexity of the laws of fluid delivery under the conditions often found.

Jan 1, 1928

By A. J. Jacobs, G. Katz

MANY of the studies of intermetallic compounds containing uranium were performed during the early 1940's under the aegis of the Manhattan Project. Subsequently, much of this work was declassified and published after 1949. In some instances this early work, completed with relatively impure materials, represents the only source of X-ray diffraction powder data available in the literature. In the case of the intermetallic compound U,Fe some discrepancies in the powder pattern exist in the literature. Since this compound has been prepared in this laboratory, it is believed that the publication of the indexed powder pattern would help clarify the conflict in the literature. In studies of the U-Fe system, Gordon and Kauf-mannl and Grogan and Clews2 independently reported the intermetallic compound U,Fe in 1950. The crystal structure was described by Baenziger, Rundle, Snow, and Wilson3 in 1950. It is isostructural with U,Mn, U,Ni, and U,Co and crystallizes in a body-centered tetragonal lattice. The lattice constants determined by Baenziger et al. are: giving an X-ray density = 17.7 g cm-3 for 4 mol per unit cell. The compound used in this study was prepared by melting a stoichiometric mixture of the constituent metals in an argon-arc furnace using a nonconsum-mable tungsten electrode. Before the argon of 99.98 pct purity was introduced into the furnace, it was passed through CaC1, to remove water vapor and afterwards through a stainless steel tube containing calcium turnings heated at 600°C for the removal of nitrogen and oxygen. The purity of the uranium used was better than 99.9 pct and that of the iron was 99.97 pct. Before and during melting a zirconium getter was used to further purify the argon atmos-

Jan 1, 1962

By H. M. Howe, E. C. Groesbeck

That the quiescence of a liquid while it is solidifying should favor the formation of columnar crystals, normal of the cooling surface, is seen readily on considering the mechanism of solidification. First, each particle of any composite liquid, whether it be an aqueous solution or a molten metal, in solidifying splits up into two parts, different in composition and hence in fusibility. One part is infusible at the existing temperature, and hence solidifies, and in general attaches itself to the inclosing walls of metal which have already solidified; A, Fig. 1. The other part is fusible at the existing temperature and hence remains molten. In the case of carbon steel, the part of each drop which actually solidifies is poorer in carbon than the drop itself was before it began to solidify, and this impoverishment of the solidifying half-drop enriches the other half-drop in carbon, and thus makes it unfreezable at the existing tern- By this mechanism there arises during solidification a "littoral" or shore layer of liquid B, Fig. 1, bathing the already solidified walls, and more fusible than either those walls or the great remaining central mass of liquid or " deep sea " C, from which it separates them. It is essential that we grasp clearly this conception of a fusible littoral molten layer coating the already solidified walls and separating them from the deep sea. Meanwhile heat is flowing rapidly outward through these walls, its escape cooling them, so that if any given particle of the deep sea metal could get past this littoral layer and come into contact with the solid walls, it would in turn solidify, and like its predecessors would split up in solidifying into a less fusible half-drop which would attach itself to those . walls and a more fusible one which would remain molten. Thus we see

Jan 1, 1920

By Robert R. Abbott

The influence of various elements in retarding or accelerating the absorption of carbon during the process of carburization is fairly well known. In general those elements which form carbides accelerate the absorption, while those which do not retard it. It has sometimes been wrongly stated that those elements which raise the temperature of the critical range increase the absorption, while those which lower this temperature decrease it. Silicon is a notable exception to this rule, for its influence is to raise the critical range but to lower the absorption of carbon. Some elements which do not form carbides have no apparent influence upon the absorption rate. Carbon itself retards the absorption rate. With a view to obtaining more exact data upon the subject the following experiments were undertaken: 208 steels of different chemical composition were selected to represent most of the types of modern constructional steels. Specimens 2 in. in diameter and 9 in. in length were weighed to milligrams. They were then packed in the special carburizing box shown in Fig. 1, and kept in the furnace for 10 hours at a temperature of 900' C. A duplicate experiment was conducted at 1,000° C. At equal intervals of time the box was rotated in the furnace so that two complete revolutions were made in the 10 hours. This precaution was taken to neutralize as much as possible any effect of unequal heating. At the end of the 10 hours the box was allowed to cool in the furnace with the doors open. The specimens were then weighed again and the increased weight (carbon) determined. In the following table are given the analyses of the various steels, together with the increased weight of carbon expressed in milligrams.

Jan 1, 1914

By L. H. de Wald, J. Walter Scott

It is usual practice in the copper industry to use open horizontal molds for casting tough-pitch copper wire bars.' A wire bar cast in this manner is partly characterized by heavy wrinkles and a comparatively deep skin of oxide on the top of the bar, corresponding to the open side of the mold. On the theory that the rough, high-oxide surface might have an adverse effect on the rolling and drawing properties of a wire bar and might account for some of the irregularities of mill behavior, several bars which had been planed to remove the wrinkled surface were processed into wire. These bars responded to mill treatment more satisfactorily than did the regular wire bars. Realizing that machining the surface of one face of each bar would not be commercially feasible, it was decided that casting the metal into a vertical mold and cropping off the pouring end would accomplish approximately the same result. Several wire bars of commercial size (250 Ib.) were so cast and processed into wire for comparative test with bars cast in the usual horizontal molds. It is the purpose of this paper to present the results obtained from this investigation, in which commercial bar sizes and processing technique were used throughout. The results show that in general copper wire bars cast vertically are superior to those cast horizontally. Experimental Procedure A horizontally cast bar and a vertically cast bar were obtained from each of several regular reverberatory furnace heats of copper which had been refined and poled to tough-pitch metal in accordance with usual methods.' Both bars were cast from the same part of the melt and within five minutes of each other, in order to produce as nearly as possible, in each case, wire bars of identical composition.

Jan 1, 1930

By A. D. Rich

THE term "bleaching clay" or "bleaching earth," as used in the oil industries, refers to clays that in their natural state, or after chemical or physical activation, have the capacity for adsorbing coloring matter from oil. There are three common types of bleaching clays: fuller's earth, activated clays, and activated bauxite. Fuller's earth, or naturally active clay, is prepared from bentonites that possess natural activity. It is not activated commercially; in fact, earths of this type ordinarily do not respond satisfactorily to acid activation. Fuller's earth is prepared in pulverized as well as granular form for use in the contacting and percolation processes, respectively. Acid-activated clays also are of bentonitic origin. The basic raw clay, however, is of a type that has a very low natural activity but is highly activable by treatment with mineral acid. Commercial acid-activated clays generally possess several times the decolorizing power (bleaching efficiency) of the best quality of fuller's earth. The former are prepared commercially only in the pulverized grade because of the difficulties in obtaining a satisfactory granular product, and hence are used only in the contact process. Activated bauxite is made by heat-treating bauxite ore, which in its natural state has very little natural activity. The commercial product is prepared in granular form for use in the percolation process on petroleum oils. For the most part, bleaching clay is used commercially in the decolorization of animal, vegetable and petroleum oils, fats and waxes. It is applied in two ways: (1) by the percolation method and (2) by the contacting method. Percolation refers to the passage of oil through a bed of granular clay whereas contacting refers to direct agitation of oil and pulverized clay followed by removal of the clay from the oil by filtration. In either case, the decolorizing effect is obtained by inti-

Jan 1, 1949

By Arthur Phillips

THE progress made in recent years in the art of dispersion-hardening has naturally led to an intensive study of alloy systems capable of yield-ing supersaturated solid solutions at ordinary temperatures. In general, the investigations have been confined to rather precise determinations of solubility limits and to experimental approaches designed to furnish more complete information regarding the rate and nature of precipitation under appropriate thermal conditions. Efforts are being made to focus more sharply on the atomic changes that are a direct consequence of the instability of the supersaturated solution. Here precision X-ray methods have come to be of considerable importance because lattice parameter measurements indicate very precisely the concentration of solute atoms in the solvent lattice. In spite of the general acceptance of parameter values as a criterion for the placing of solubility limits, it may be suggested that no thorough appraisal has been made of the several factors that conceivably may affect such measurements. More specifically, little attention has been devoted to the significance of surface energy conditions, specimen size and method of preparation, with par-ticular regard to the genesis of the grains and the surface concentration changes as a consequence of heat treatment and etching. Stenzel and Weerts1 recently published the results of a detailed study of precipitation reactions in aluminum-rich copper alloys. They found that, although copper lowers the lattice constant of aluminum, a 5 per cent copper alloy quenched from 150° and 225° C. had parameter values unquestionably higher than that of pure aluminum. Their results seem to substantiate, at least qualitatively, the earlier work of von Göler

Jan 1, 1934

By D. L. Katz

The critical phenomena have been studied during the past century but our knowledge of the critical temperatures and pressures of complex hydrocarbon mixtures still is very limited. The critical temperatures and pressures of pure substances have been examined in large num-bers,20 and in great detail.11,17 No experimental determinations of the critical phenomena have been reported on such complex hydrocarbon systems as a reservoir fluid. The critical temperature is defined by Taylor18 as follows: "there is some temperature for each gas above which the gas cannot be liquefied. This temperature is called the critical temperature." The critical pres-sure of a pure substance is the vapor pressure at the critical temperature. It should be noted that these definitions refer to a given substance in the pure state and do not mean that the pure substance cannot be liquefied in the presence of a second constituent. The normal procedure for obtaining the critical temperature of a substance is to heat it in a glass tube 1,20 under pressure until the meniscus between the liquid and vapor phase disappears, although other methods, especially for mixtures, have been used. 11,14 However, when considering oil and gas reservoirs, it is more enlightening to consider a critical phe-nomenon that occurs when a mixture of oil and gas are compressed at a reservoir temperature until the meniscus disappears because the two phases become equal in composition. This conception, along with erroneous applications of the definition of the critical phenomena of a pure substance to that pure substance when it is part of a complex mixture, has caused confusion even among persons familiar with the classical theories.

Jan 1, 1938

By T. B. Counselman

AFTER several years study, the Universal Atlas Cement Co. decided to rebuild its plant at Leeds, Alabama. The entire old plant, which was to operate during the new construction, was then to be scrapped with the exception of two kilns. The quarry was to be mechanized, new and larger kilns installed, with the most modern type of equipment all through the plant. Raw grinding operations at all of the Universal Atlas plants were dry. However, the dust hazard of this operation and the growing emphasis on occupational diseases made wet grinding attractive. Coal at Leeds is cheap, so that a slightly higher coal practice was unimportant. Power was cheap, so that waste-heat boilers were not desirable. Since new kilns were to be installed, these could be made long enough to make filters unnecessary. Wet raw grinding could be either the old practice of open-circuit compartment mills or closed-circuit grinding in accordance with metal-lurgical practice. The latter saved power and steel wear and saved initial investment. This had been demonstrated in cement plants. Also, the elimination of tramp oversize was a most important advantage. Ease of chemical control was another factor. Blending in the thickener, with elimination of slurry mixers had been found practicable. Therefore, if wet raw grinding were used at all, the advantages were clearly in favor of closed-circuit grinding. Detailed layouts of the most modern possible closed-circuit dry-grinding plant and of a closed-circuit wet-grinding plant were prepared, and careful estimates were made of initial invest-ment and operating costs. Full consideration of all the factors involved resulted in a decision to install wet closed-circuit grinding.

Jan 1, 1939

By Robert L. Braun, Arthur E. Lewis

A contained nuclear explosion is proposed to produce a chimney of broken ore well below the water table. After the chimney is filled with water and reaches hydrostatic equilibrium, oxygen, under pressure, is introduced near the bottom of the mass of broken rock. The increase in solubility of oxygen at high hydrostatic pressure is sufficient to initiate the oxidation of the primary sulfides, chalcopyrite and pyrite. The oxidation and dissolution of these sulfides produces enough heat to increase the temperature of the ore and water in the chimney as much as 100° to 150°C. The rate of dissolution of chalcopyrite exposed to oxygen-saturated solutions becomes so rapid under these conditions that the rate of copper extraction becomes limited by the accessibility of chalcopyrite to the solutions. Means of solution control and distribution of oxygen in the chimney have been examined in some detail. A calculational model utilizing experimentally determined solubility rates is utilized to estimate the temperature rise in the chimney and the rate of copper recovery as a function of initial temperature, sulfide content of ore, and size of ore particles. It is concluded that the high pressure and high temperature obtainable in a large ore mass broken by nuclear explosives promise the rapid and economic recovery of minerals not considered soluble by conventional in-situ leaching methods. The method should be broadly applicable to the kinds of deep deposits that must be depended on for future production and with minimum disruption of the environment.

Jan 1, 1974

CONTENTS PAGE ANDERSON, ROBERT J., and ENOS, GEORGE M.-Corrosion of Brass as Affected by Grain Size. Discussed by Henry S. Rawdon, Robert J. Anderson, Francis B. Coyle, William B. Price, and W. R. Webster 1 RAWDON, HENRYS., and MUTCHLER, WILLARD H.-Effect of Severe Cold Working on Scratch and Brinell Hardness. Discussed by W. H. Bassett, John Livermore Christie, John R. Freeman, Jr., W. R. Webster, William B. Price, Norman B. Pilling, D. J. McAdam, Jr., F. G. Smith, Zay Jeffries, F. E. Carter 3 WILLIAMS, ROBERT S., and HOMERBERG, VICTOR 0.-Relation of Heat Treatment to the Microstructure of 60-40 Brass. Discussed by 0. W. Ellis 14 Corrosion of Brass as Affected by Grain Size Discussion of the paper of ROBERT J. ANDERSON and GEORGE M. ENOS, presented at the New York Meeting, February, 1924, and issued as Paper No. 1282, with MINING AND METALLURGY, December, 1923. HENRY S. RAWDON,* Washington, D. C. (written discussion).-So numerous and so varied are the factors that affect the corrosion of metals that particular care is necessary in corrosion tests to eliminate so far as possible all extraneous factors. It appears to the writer that the question may well be asked as to whether all the necessary precautions have been observed in this investigation. It may be that the points to be mentioned were considered by the authors and found to be insignificant; however, there is nothing in the report to show this.

Jan 5, 1924

By Walter Miller

Any annual review of engineering progress in petroleum refining must of necessity include many features mentioned in earlier reviews. Advances do not spring mushroom fashion to wide acceptance overnight, but rather resemble rolling snowballs, gathering size and velocity as they progress. The new ideas of one year develop through the course of scattered adoption and testing during following years, to be ultimately discarded or to become an integral part of refinery engineering and operation. Polymerization and Cracking As an illustration, the publicity given to the polymerization and cracking of petroleum gases during the year has given many the impression that this is a new art. But patent and technical literature have disclosed active work on the problem dating back a decade or more and a unit capable of making 100 bbl. a day of polymer gasoline was constructed as early as 1930. Important strides have been made during 1935 looking to the more general commercialization of available processes, and some four important groups are furthering this work. In addition to the production of liquid products for inclusion as a constituent of commercial motor fuel, polymerization has also been a factor leading to the installation of a plant at the Houston refinery of The Shell Petroleum Corporation for manufacturing isooctane for aviation use, by making available dibutylene for catalytic hydrogenation Polymerization is not confined to unsaturated hydrocarbon gases as a source of raw material, and has been extended to include a preliminary decomposition of normal saturated gases under suitable heat and pressure conditions into the unsaturated types, which can then be used as raw material for the polymerization process. Thus there is opened up the possibility of eventually using large quantities of natural gas in the manufacture of high-grade motor fuels, although the early commercial growth will be largely on cracking still gases for economic reasons. Such utilization will result in a somewhat lowered drain on crude-oil reserves and a partial elimination of the

Jan 1, 1936

By J. W. Halley

Copper has frequently been recommended as an alloying element for steel and the precipitation-hardening of steels containing from 1 to 2 per cent copper has been studied by a number of investigators. The straight copper steels, however, have not been used extensively and little advantage has been taken of the precipitation-hardening of complex steels containing appreciable amounts of copper. It is difficult to produce a satisfactory surface on the straight copper steels and undoubtedly this has discouraged their use. During recent years a number of steels containing enough copper to make them susceptible to precipitation-hardening have been put on the market. These steels belong to the group usually referred to as "low-alloy high-tensile " steels. They were designed for use in the " hot-rolled" condition; transportation equipment and large structures that cannot be readily heat-treated have been their chief application. Little emphasis has been placed on the possibility of strengthening those containing substantial amounts of copper by precipitation-hardening. The present investigation was undertaken to determine the precipitation-hardening characteristic of one of the "low-alloy steels." Previous Work The first complete study of the effect of time and temperature on the precipitation-hardening of plain copper steels was made by Nehll in 1930. At about the same time Bucholtz and Koster2 studied copper-chromium steels but did not determine the relation between time and temperature to produce maximum hardening. Later, Smith and Palmer3 determined the rate of hardening at various temperatures for two I per cent copper steels containing different amounts of carbon. Their tests indicated that the higher carbon content decreased the rate of hardening. They made tests on many steels containing other alloying elements in addition to copper, but did not determine the time-temperature relationship for maximum hardening for any of the complex steels. Norton,4 in studying the limit of solid solubility of copper in iron, determined the time for maximum hardening of a 2.06 per cent Cu iron

Jan 1, 1940

By Walter Miller

Any annual review of engineering progress in petroleum refining must of necessity include many features mentioned in earlier reviews. Advances do not spring mushroom fashion to wide acceptance overnight, but rather resemble rolling snowballs, gathering size and velocity as they progress. The new ideas of one year develop through the course of scattered adoption and testing during following years, to be ultimately discarded or to become an integral part of refinery engineering and operation. Polymerization and Cracking As an illustration, the publicity given to the polymerization and cracking of petroleum gases during the year has given many the impression that this is a new art. But patent and technical literature have disclosed active work on the problem dating back a decade or more and a unit capable of making 100 bbl. a day of polymer gasoline was constructed as early as 1930. Important strides have been made during 1935 looking to the more general commercialization of available processes, and some four important groups are furthering this work. In addition to the production of liquid products for inclusion as a constituent of commercial motor fuel, polymerization has also been a factor leading to the installation of a plant at the Houston refinery of The Shell Petroleum Corporation for manufacturing isooctane for aviation use, by making available dibutylene for catalytic hydrogenation Polymerization is not confined to unsaturated hydrocarbon gases as a source of raw material, and has been extended to include a preliminary decomposition of normal saturated gases under suitable heat and pressure conditions into the unsaturated types, which can then be used as raw material for the polymerization process. Thus there is opened up the possibility of eventually using large quantities of natural gas in the manufacture of high-grade motor fuels, although the early commercial growth will be largely on cracking still gases for economic reasons. Such utilization will result in a somewhat lowered drain on crude-oil reserves and a partial elimination of the

Jan 1, 1936

By N. A. D. Parlee, I. D. Shah

ThIS reports on some work done on the solubility and diffusivity of oxygen in liquid silver. Solubility. Improvements in the measurement of the solubility of oxygen in silver and silver alloys were made because precise data were needed for calculating diffusion coefficients of oxygen in these alloys. The apparatus and the procedure used were similar to those of Parlee and Sacris.' The main improvement was in the temperature-measuring technique. A MV30 mullite protection tube containing a calibrated Pt-Pt, 10 pct Rh thermocouple was inserted in the reaction tube from the top through a vacuum-tight swage-lok fitting. The protection tube was well-immersed in the liquid silver, which was heated by induction. A Leeds and Northrup potentiometer was used in connection with the thermocouple. All runs reported were made at 1 atm. The temperature range investigated varied from 940" to 1200°C. The ternary point in Ag-0 phase diagram2 is at 939°C and 0.32 wt pct O. This point was reinvestigated using the above-described apparatus and was found to be at 939°C and 0.315 wt pct 0. It was determined by observing the sudden evolution of oxygen at this point while the solubility measurements were made. The point was easily reproducible if precautions were taken to keep the liquid silver essentially in equilibrium with oxygen and to lower the temperature very slowly. All of the results of this new solubility investigation are plotted in Fig. 1. They are represented by the "least-squares" line shown in the figure and the following equation for solubility at po2 = 1 atm: log% O =695.4/T - 1.086 This equation differs only slightly from that proposed by Parlee and sacrisl and that of Diaz, Masson, and Richardson.3 The points of Parlee and Sacris, using an optical pyrometer, are shown for comparison.

Jan 1, 1968

By Mary Louise Theodore, R. G. Aspden, D. A. Colling

T RACES of sulfur have a marked influence on the physical and mechanical properties of many iron-base alloys. The commonly used combustion method for the determination of sulfur content is not accurate enough at the 50 ppm level by weight and below to be useful in determining the influence of sulfur. Kriege and Wolfe' have described a method for the determination of sulfur in iron alloys in which the sulfur is evolved as hydrogen sulfide followed by reaction with N, N-dimethyl-p-phenylenediamine, and iron (111) to form methylene blue which is measured spectrophoto-metrically. This method of determining sulfur has been used to study the activity of sulfur in Fe-Si-S alloys,' but has not been previously applied to the determination of sulfur in Fe-Ni alloys because of the insolubility of nickel in dilute hydrochloric acid. Dissolution of nickel in dilute hydrochloric acid, however, can be greatly accelerated by the addition of a small amount of platinic chloride.3 By combining these two techniques in a procedure in which 0.005 pct platinic chloride in 1:l hydrochloric acid is used as the dissolving fect on the strength of the material. However, ductility is influenced by the presence of discontinuous precipitation. In Fig. 5, percent elongation data at room temperature and 1400°F is shown for two sets of specimens of Waspalloy which were solution heat treated at 1950°F and either quenched or slow cooled to the aging temperature and then aged for 100 hr at 1292" and 1598ºF, respectively. At room temperature the existence of a discontinuous precipitation cell at grain boundaries (see data point marked by arrow) has no apparent effect on ductility. However, at elevated temperatures a pronounced lowering of ductility occurs when discontinuous precipitation has occurred in the specimen. It would appear that the morphology of discontinuous precipitation "cells" at grain boundaries would be highly conducive to the initiation of cracks which in turn lead to premature "grain boundary" failure.

Jan 1, 1970

By Charles Baskerville

Shales containing "kerogen," or bituminous matter, which on destructive distillation yield oily and tarry matters resembling petroleum are here designated as oil-shales. They differ from oil-bearing shales from which petroleum may be obtained by so-called mechanical means. The educts obtained by the destructive distillation resemble some or all the varieties of petroleum, depending on the character of the shale and the mode of treatment. Some shale oils have a paraffin base, some an asphaltic base, or a combination; some run high in sulfur compounds. The methods of refining and cracking, therefore, are essentially the same as are used in refining petroleums. In 1860, in this country, over fifty companies were successfully distilling various natural bituminous materials for the production of " coal oil," used for illuminating purposes. The discovery of petroleum and the failure of these companies to save and utilize the valuable byproduct, ammonia, brought about their inevitable doom. Prior to that time, more or less successful efforts were made to produce from the shales of Scotland oils for illuminating and heating purposes. Competition of native petroleum from the United States early eliminated some of these companies and with the entrance of oil from the Russian and other fields into the world's markets, the Scottish oil-shale industry underwent serious and trying experiences until, in 1916, only four (Scottish) were paying concerns. These survived only through energy and the application of skill in saving valuable byproducts. A few companies have successfully operated in France and New Zealand. The Canadian Government showed active interest in the New Brunswick shales, which exist in quantity and are more valuable than the Scottish shales. The retarded development of that valuable asset of the Province of New Brunswick was most unfortunate, especially when the product was so much needed in the prosecution of the war. The economic success of a shale-oil industry depends on the following factors:

Jan 1, 1921