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By P. A. Tucker, C. R. Hudgens, D. E. Etter, D. L. Roesch, D. B. Martin

The equilibrium phase diagram of the Pu-Cd system is presented based on data obtained by differential thermal analysis, metallography, and electron-microprobe X-ray analysis. Liquidus temperatures range from 320° to 934°C. The system contains one congruently melting compound, PuCd, (945°C), and three incongruently melting compounds, PuCd, (800°C), PuCd, (730°C), and PuCd11 (410°C). A liquid-miscibility gap extends from 2 to 60 at. pet Cd with the monotectic reaction isotherm at 910°C. INTEREST in the potential use of plutonium alloys as reactor-fuel materials has prompted investigation of the phase equilibria in plutonium binary systems. A cursory investigation of the phase equilibria in the Pu-Cd binary system was conducted by differential thermal analysis (DTA), metallography, and electron-microprobe X-ray analysis (EMX). Extensive solid solubility of cadmium in both e and 6 plutonium was predicted1 based on atomic radii and electronegativities. Liquid immiscibility between these two elements was also predicted based on Mott's extension of Hildebrand's method. In the only previous investigation of the Pu-Cd system,2 two intermetallic compounds, PuCd11 (incon-gruent melting point 406°C) and PuCd8, were identified. EXPERIMENTAL The plutonium metal used in this work had a total impurity content of 500 ppm; the major impurities were: carbon (215 pprn), silicon (75 ppm), iron (60 ppm), nickel (40 ppm), and aluminum (25 ppm). The cadmium was reagent grade with a purity of 99.99 pet. The DTA technique for the study of plutonium alloys was previously described in detail.3 The alloys to be studied were prepared in tantalum DTA specimen capsules which were sealed by inert-gas welding. The alloys were homogenized in the liquid state in these sealed capsules which prevented the loss of cadmium by vaporization. Only the thermal arrests in the DTA heating curves were used to define the transformation temperatures of the system since supercooling affected many of the results during cooling. After the alloys were analyzed by DTA, the same alloys were used for the metallographic studies. Metallographic examinations were conducted in the manner described for plutonium alloys., No reaction was detected between the alloys and the tantalum capsules. Alloys for EMX analysis were placed in metallographic mounts together with specimens of unalloyed plutonium and cadmium which served as standards. The samples were highly polished but unetched. No protective coatings were applied to the surfaces of these radioactive specimens. Such coatings are detrimental to the excitation conditions and have been found to be unnecessary for the control of radioactive contamination. RESULTS The results of the DTA studies are presented in Table I. The phase diagram, constructed from these data plus the metallographic and EMX results, is presented in Fig. 1. The congruently melting compound, PuCd2, was identified by the occurrence of a maximum melting point (945°C) at 33.3 at. pet Pu-66.7 at. pet Cd and by the presence of a single phase in this composition.

Jan 1, 1965

By N. Van Wingen, Norris Johnston

Laboratory flood pot testing of California sands has progressed to a considerable extent in the past 18 months. Flood evaluations have been carried out on over 200 large core samples. Many of these were heavy oil sands of high permeability and completely unconsolidated in nature. The oil frequently formed a bank, though some of the oil was recovered in the subordinate phase of the flood, by viscous drag. Flood pot recoveries as high as 1400 bbl/acre ft have been recorded. Reservoir analysis suggests a conformance factor of 0.4 to reduce laboratory recovery to probable field practice. Oils with viscosities up to 1800 cp have been successfully handled in flood pot evaluations. The shallow, loose sands are not well adapted to the application of- high pressures to offset the high viscosities. INTRODUCTION Secondary recovery may be said to have started 60 years ago when accidental floods occurred in the Bradford sand in Pennsylvania. About 1921 artificially conducted water drives came into extensive use and since that time the great Bradford field has been almost completely subjected to water flooding. During the last 30 years, most of the known medium and deeper production in California has been discovered and is being exploited by primary recovery methods supplemented in some instances by high pressure gas injection. The California area is just beginning to feel the need for secondary recovery in view of an unprecedented market demand and the rapidly rising cost of new pool discoveries. With the presently recognized desirability of secondary recovery in California, there must also be appreciated a number of serious differences between the water flooding problems here as compared to the territory east of the Rockies. California sands are generally thicker, and are frequently soft and argillaceous. The oils are often heavier and asphaltic. Much of the oil is below 15°API, occurs at shallow depth, is cool and free from appreciable dissolved gas, which results in relatively high reservoir oil viscosity. Secondary recovery is particularly beneficial where primary recovery has been poor and where no natural water drive exists. These conditions apply particularly to the heavy, shallow, clean production from soft, often argillaceous California sands so abundantly found at depths less than 1500 feet. Often, too, there is a totally insufficient supply of water of satisfactory quality to inject at a reasonable cost. Also, the crude oils are priced far below the premium Bradford crude. Although these and a number of minor problems beset the operator desirous of starting secondary recovery, great progress has been made in the past few years in finding how to adapt previous Mid-Continent and Eastern experience to water flooding in California. There are about nine projects for subsurface injection of water which can be said to classify as secondary recovery operations. Subsurface water disposal would so classify when the sand receiving the water is a nearby oil producer, as is often the case. When water is injected subsurface into a barren sand, the operation does not classify as secondary recovery. Several of the most active operators avail themselves extensively of preliminary engineering and laboratory work to guide their decisions, while others enter small scale flooding operations directly in the field. It is the laboratory work pertinent to several of the California secondary recovery projects that this paper discusses. PURPOSES OF LABORATORY FLOODING TESTS Experience in areas where water flood operations have been carried out has indicated that careful engineering planning is an important requisite for subsequent economically successful field operation. Floods that fail are more frequently those where operations were instigated without a prior engineering investigation to determine the effectiveness of the injection fluid as an oil displacing medium. Laboratory data are essential in the evaluation of an oil property for secondary recovery possibilities. Success or failure of secondary operations can under certain special circumstances be determined directly by cores and their subsequent routine analysis. This is particularly the case where flushing of the cores in the course of coring is negligible and where the results of the analysis can be compared with existing secondary recovery operations. Where these conditions cannot be' fulfilled, the application of core analysis is more limited. In such event, the results obtained by water flooding core samples in the laboratory have been found to be of prime importance. Cores may be flooded "raw" as taken from the well or in the event flushing and depletion of the cores in the process of drilling are major factors the fluid content may be artificially restored prior to the flooding. Laboratory studies should also be made to determine the suitability of the water selected for injection. Thus interaction between injected and formation water may cause precipitates to be formed which may plug the sand. Even more important, especially to California operations, is the possibility of the hydration of formation clays by the injection water. The aims of flood pot and associated tests are basically to determine the residual oil saturation after flood, the water-oil throughput ratio and to establish whether an oil bank is formed. Additional information which can be obtained from flood pot tests pertains to the pressure differential required to effect displacement, the relative permeability to oil in the oil bank and the relative permeability to water in the watered out region behind the bank.

Jan 1, 1953

By Max Heberlein, R. P. E. Hermsdorf

The electrolytic refining of metals for the removal of undesirable impurities has become a recognized necessity in the nonferrous field. Copper, lead, zinc, nickel, silver and gold have been produced in this manner for years. The United States Metals Refining Co., realizing that considerable quantities of lead and tin could be made available to the trade if a satisfactory method of purification of these metals could be established, decided to investigate the possibilities of electrolytic solder. In cooperation with Dr. Edward F. Kern, of the School of Mines at Columbia University, the company developed a process of electrolytic refining of lead-tin alloys using a tin-lead fluosilicate electrolyte. A pilot plant was installed in November 1927, and the commercial unit was put in October 1929. Since that time thousands of tons of electrolytic solder have been produced in this plant and consumed by all branches of industry that use solder. Older Methods of Producing Solder In the early days practically all solder was made by melting together virgin lead and tin in the proper proportions to meet specifications; then the solder was cast into the commercial shapes required. Today the base of most solders comes from scrap or secondary materials. Ordinarily solder is produced from secondary materials either by sweating solder-bearing scrap or by smelting lead and tin-bearing drosses, residues and similar materials. When solder is produced from scrap by sweating, clear solder is collected directly. It is then given some kind of kettle refining and usually blended to specification with virgin metals before it is cast into finished shapes. In producing solder from drosses and residues, the materials are usually first given a reducing smelting treatment from which a crude solder is obtained. This crude solder may be refined in several ways, but usually the first step is a furnace liquation to remove the bulk of the copper, which is followed by one of the more or less complicated methods for the removal of antimony and other impurities.

Jan 1, 1937

By George Otis Smith

In the utilization of natural resources owner, operator, and consumer* should share the attendant benefits. Development needs to be planned under terms recognizing fully the interests of all concerned, for ally undue advantage given to any one of these participants is apt to involve even greater and disproportionate injury to one or both of the others. For this reason it is well to preface any consideration of needed reforms in legislation affecting the disposition of public land with a survey of certain fundamental principles that determine the general conditions of a11 land transfers preliminary to development, utilization, and production. The disposition of any undeveloped natural resource, whether timber, oil, coal, or water power, as a transaction to which land owner and prospective developer are parties, must be based in theory upon a division of expected returns.' Whatever the terms of such disposition, neither party can reasonably ask for anything other than an equitable division of the returns. Under this analysis three and only three questions need to be discussed; namely, what are those profits, how is this division to be accomplished, and what is the equitable basis of division ? The answer to the third question should probably be found by applying to the problem the principles of theoretical sociology, and the question need not be mentioned further at this time, inasmuch as it does not involve the practical considerations to be kept in mind in connection with the other questions, which are concerned with only the measure of returns and their division. That is to say, whether the land owner's equity is to be stated as 95 per cent, ox as 6 per cent, of the profits attending the development of the particular resource, no change would be necessary in the method to be adopted of arriving at the closest approximation of the prospective total profit. If on this basis we now compare the two methods of disposing of

Jan 1, 1915

By V. R. Garfias, H. J. Hawley

FoR a number of years the senior author has been interested in the various geologic and engineering problems involved in the development of the petroliferous districts of northeastern Mexico, having in a previous paper* endeavored to present a summarized statement of the information relating to the geology and soil resources of this region. Of the many interesting geologic phenomena, perhaps those which have been the object of most speculation relate to the igneous intrusions which, in places, have a controlling influence on the accumulation of oil in commercial quantibies, a relationship which has been tentatively explained by various observers with as many interestingly different views. The authors of the present paper aim to record, in the course of a general discussion of the various viewpoints, some additional data, and present further tentative conclusions with a view to rounding out an up-to-date summary of the subject. The greater part of the area in question lies in the State of Vera Cruz, only a northwest fraction being in the State of San Luis Potosi. Vera Cruz is bounded on the north by the State of Tamaulipas, the northernmost of the Mexican States along the Gulf. The topography of the States of Tamaulipas and Vera Cruz and of Texas and Louisiana to the north, is controlled by the Gulf coastal plain which in northern Vera Cruz has an average width of about, 60 miles, the transitional topography between that of the rugged Banks of the Sierra and the lowlands of the coast being made up of a series of terraces and irregular hills and valleys. Geology and StRucture The greater part of the mainland of Mexico is made up of Tertiary and later effusive rocks and of sedimentaries of Cretaceous age. The igneous rocks form a belt from 150 to 300 miles wide, spurs of which shirt

Jan 1, 1918

By W. M. Peirce

Commencing in 1922, each year a lecture has been presented to the Institute of Metals Division at this February meeting. The range of subjects has been very- broad. Some speakers have dealt with the most advanced work in the very heart of the science of physical metallurgy. Others have stimulated our imaginations by discussing the most recent progress in related fields of science. Others have told us of the latest art, which is at any moment of greater practical importance than the latest science, of metals. I feel that this broad precedent in the choice of subjects will justify my choosing to talk about some of the prosaic details of how, during the last generation, industry has effectively organized research to accelerate progress in our own and all other fields of science and related art. A number of years ago I visited one of this country's well-known research laboratories and had the pleasure of chatting for a few minutes with its equally well-known director. Being particularly interested at the time in the organization problems connected with industrial research, I broached that subject. My host stated in effect that he didn't believe in organized research. He was, of course, resorting to a rhetorical hyperbole. to pain: out the danger of overorganization which can so easily drift into regimentation and destroy individual initiative. Actually nearly all of us, much as we cherish our personal freedom of action, believe in organization because the history of progress in every field of human activity has been a history of men learning to work together, to cooperate, to create an efficient division of labor. We use organization to achieve this coordination. At the same time our form of organization must not stifle individual initiative or it will prove a deterrent rather than an aid to accomplishment. Research, too, must be organized for greatest achievement but especial skill and care are perhaps needed to avoid stifling the initiative of the individual workers. I have, of course, followed with keen interest and much benefit the vast amount . that has been said and written on this subject in the past twenty years but I still find new stimulation in discussions with my good friends working in this field. It is my hope that this discussion may serve a like purpose. It would be ungracious not to make due acknowledgment to the many able contributors to this particular phase of human progress, but their very number and the great volume of their writing makes it impossible to trace to any one individual a particular significant and valuable idea. I shall content myself therefore with this general acknowledgment and with acknowledgment of the specific debt that every research man owes to those who have so ably kept before the public, and in particular before industrial executives, the place of research in the modern scheme of things' Because of the legitimate publicity thus given to research, the day is past when any

Jan 1, 1944

By W. M. Peirce

Commencing in 1922, each year a lecture has been presented to the Institute of Metals Division at this February meeting. The range of subjects has been very- broad. Some speakers have dealt with the most advanced work in the very heart of the science of physical metallurgy. Others have stimulated our imaginations by discussing the most recent progress in related fields of science. Others have told us of the latest art, which is at any moment of greater practical importance than the latest science, of metals. I feel that this broad precedent in the choice of subjects will justify my choosing to talk about some of the prosaic details of how, during the last generation, industry has effectively organized research to accelerate progress in our own and all other fields of science and related art. A number of years ago I visited one of this country's well-known research laboratories and had the pleasure of chatting for a few minutes with its equally well-known director. Being particularly interested at the time in the organization problems connected with industrial research, I broached that subject. My host stated in effect that he didn't believe in organized research. He was, of course, resorting to a rhetorical hyperbole. to pain: out the danger of overorganization which can so easily drift into regimentation and destroy individual initiative. Actually nearly all of us, much as we cherish our personal freedom of action, believe in organization because the history of progress in every field of human activity has been a history of men learning to work together, to cooperate, to create an efficient division of labor. We use organization to achieve this coordination. At the same time our form of organization must not stifle individual initiative or it will prove a deterrent rather than an aid to accomplishment. Research, too, must be organized for greatest achievement but especial skill and care are perhaps needed to avoid stifling the initiative of the individual workers. I have, of course, followed with keen interest and much benefit the vast amount . that has been said and written on this subject in the past twenty years but I still find new stimulation in discussions with my good friends working in this field. It is my hope that this discussion may serve a like purpose. It would be ungracious not to make due acknowledgment to the many able contributors to this particular phase of human progress, but their very number and the great volume of their writing makes it impossible to trace to any one individual a particular significant and valuable idea. I shall content myself therefore with this general acknowledgment and with acknowledgment of the specific debt that every research man owes to those who have so ably kept before the public, and in particular before industrial executives, the place of research in the modern scheme of things' Because of the legitimate publicity thus given to research, the day is past when any

Jan 1, 1944

By R. A. Morse, W. O. Keller

The properties of limestone reservoir rocks such as the distribution and degree of continuity of the pore systems, and the relative volumes and permeabilities of the systems making up the complex cause large variations between performance of individual limestone reservoirs and their susceptibility to secondary recovery methods. The effects of these factors on the mechanism of fluid flow cannot be adequately evaluated with presently developed concepts, laboratory data, and geological information. The observance and interpretation of the performance of individual limestone reservoirs provides, at present, the most adequate approach for evaluating the integrated effects upon performance of the many. now immeasurable variations in the properties of limestone reservoirs. INTRODUCTION The development and application of techniques for increasing the efficiency of oil recovery from natural reservoirs is a problem of primary importance to the industry. During the past several years, a great deal of effort has been expended by the technical personnel of the industry toward the improvement of present known methods of oil recovery. and evaluating the factors which control the susceptibility of particular reservoir types to economic application of secondary recovery methods. Providing adequate and accurate laboratory data on the properties of the reservoir rock and its contained fluids. together with good production statistics, are available, methods have been evolved for estimating with reasonable accuracy the performance of an oil reservoir under either continued natural depletion or conditions imposed by introducing additional displacing fluid into the reservoir from an extraneous source through the injection of gas and/or water. The susceptibility of limestone reservoirs to secondary recovery by gas injection is very much dependent upon gas-oil relative permeability relationships for the reservoir in question. In a rock formation in which the porosity is of the intergranular type such as is found in sand stones and some non-fractured dolomites, a representative sample of the pore structure can be obtained in a small core plug. In this type of reservoir, it has been shown that relative permeability data obtained from laboratory experiments can be Properly applied to evaluate the flow relationships actually observed during the depletion of a reservoir. In addition, a good idea of the fraction of the reservoir which will be swept by the injected gas may be obtained from the spacing pattern used and the permeability profile of cored wells. From these data, it has been demonstrated that reliable estimates of performance and recoveries under gas injection operations can be made for reservoirs in which the Porosity is of the intergranular type. Limestone reservoirs on the other hand often present much more complex problems. One reason that the performance of limestone reservoirs is so variable is that there may be, in reality. two or more pore systems, the integrated performance of which will depend upon the physical properties of each system and their inter-relationship. For instance, in a limestone reservoir, the main pore structure, as far as void spaces for storage of hydrocarbons is concerned, may be represented by the intergranular openings of the rock. Usually in limes and dolomites, the intergranular pore openings are very small and the matrix permeabilities extremely low. Often, as in the case of Many dolomite and oolitic lime reservoirs, this is the only pore system, and performance is observed to be very similar to that of a sand stone of similar permeability. However, in the great majority of' the limestone reservoirs, there is present, in addition to the intergranular pore system, a complementary system of openings caused by fracturing or solution.',' The openings in the latter system are usually many times more permeable than the intergranular pore system due to their much larger size, and may contribute almost all the fluid carrying capacity of the formation, even though their volume may be a very small part of the total pore space in the reservoir. Obviously, the performance of such a complex under either primary or secondary control will deend upon the distribution and degree of continuity of both systems, the relative volumes and permeabilities of the

Jan 1, 1949

By R. A. Morse, W. O. Keller

The properties of limestone reservoir rocks such as the distribution and degree of continuity of the pore systems, and the relative volumes and permeabilities of the systems making up the complex cause large variations between performance of individual limestone reservoirs and their susceptibility to secondary recovery methods. The effects of these factors on the mechanism of fluid flow cannot be adequately evaluated with presently developed concepts, laboratory data, and geological information. The observance and interpretation of the performance of individual limestone reservoirs provides, at present, the most adequate approach for evaluating the integrated effects upon performance of the many. now immeasurable variations in the properties of limestone reservoirs. INTRODUCTION The development and application of techniques for increasing the efficiency of oil recovery from natural reservoirs is a problem of primary importance to the industry. During the past several years, a great deal of effort has been expended by the technical personnel of the industry toward the improvement of present known methods of oil recovery. and evaluating the factors which control the susceptibility of particular reservoir types to economic application of secondary recovery methods. Providing adequate and accurate laboratory data on the properties of the reservoir rock and its contained fluids. together with good production statistics, are available, methods have been evolved for estimating with reasonable accuracy the performance of an oil reservoir under either continued natural depletion or conditions imposed by introducing additional displacing fluid into the reservoir from an extraneous source through the injection of gas and/or water. The susceptibility of limestone reservoirs to secondary recovery by gas injection is very much dependent upon gas-oil relative permeability relationships for the reservoir in question. In a rock formation in which the porosity is of the intergranular type such as is found in sand stones and some non-fractured dolomites, a representative sample of the pore structure can be obtained in a small core plug. In this type of reservoir, it has been shown that relative permeability data obtained from laboratory experiments can be Properly applied to evaluate the flow relationships actually observed during the depletion of a reservoir. In addition, a good idea of the fraction of the reservoir which will be swept by the injected gas may be obtained from the spacing pattern used and the permeability profile of cored wells. From these data, it has been demonstrated that reliable estimates of performance and recoveries under gas injection operations can be made for reservoirs in which the Porosity is of the intergranular type. Limestone reservoirs on the other hand often present much more complex problems. One reason that the performance of limestone reservoirs is so variable is that there may be, in reality. two or more pore systems, the integrated performance of which will depend upon the physical properties of each system and their inter-relationship. For instance, in a limestone reservoir, the main pore structure, as far as void spaces for storage of hydrocarbons is concerned, may be represented by the intergranular openings of the rock. Usually in limes and dolomites, the intergranular pore openings are very small and the matrix permeabilities extremely low. Often, as in the case of Many dolomite and oolitic lime reservoirs, this is the only pore system, and performance is observed to be very similar to that of a sand stone of similar permeability. However, in the great majority of' the limestone reservoirs, there is present, in addition to the intergranular pore system, a complementary system of openings caused by fracturing or solution.',' The openings in the latter system are usually many times more permeable than the intergranular pore system due to their much larger size, and may contribute almost all the fluid carrying capacity of the formation, even though their volume may be a very small part of the total pore space in the reservoir. Obviously, the performance of such a complex under either primary or secondary control will deend upon the distribution and degree of continuity of both systems, the relative volumes and permeabilities of the

Jan 1, 1949

By Charles Morgan

AN increased demand for brown iron ore in the Birmingham district during the past 18 months has caused renewed activity both in prospecting and mining these ores. In recent years the production in Alabama has ranged from 41,559 tons in 1932 to 639,351 tons in 1928. During the last 9 years about 83 per cent of the total brown ore produced in the United States has come from Alabama (Tables 1 and 2). PROSPECTING Two methods of prospecting are used in this district: (1) test pits, (2) churn-drilling. Usually there is certain quite definite information on an area to be prospected; some of the indications are float ore suck as small gravel or small and large boulders known as "dornicks” scattered over the surface, and ore exposed by erosion in gulleys and ravines, which have cut or eroded through the overburden. Often these natural erosions furnish an indication of the thickness of the ore and to some extent of the area of the ore body. Deposits of brown ore are very irregular both in thickness and extent. Deposits are often lens-shaped or long narrow leads, some of which may be parallel and separated from one another by sand, clay or gravel. The bottom-the footwall-is also very irregular. This footwall is usually lime clay-disintegrated limestone, locally called "white horse," which usually is found at a depth of 6 in. to 20 ft. overlying the limestone. At some places sand and gravel is found under the ore instead of clay. No ore is found under the lime clay, although often the ore has sunk or slumped and is found in the upper portion of this clay, as at some of the Sloss workings at Russellville. The origin of these ores has been discussed by Major E. C. Eckel and Dr. E. F. Burchard in U. S. Geological Survey Bulletin 400, and recently the latter has done further work on ores in the Russellville district, of which reports undoubtedly will be published.

Jan 1, 1937

By Paul Merica

ALTHOUGH nickel was discovered and isolated as early as 1750 and its valuable properties recognized, many years passed before it was used commercially for wire, sheet, rods, etc., in the pure form. This was due partly to its high cost at that time and partly to the fact that it was not possible to refine and cast nickel into ingots sufficiently malleable to be amenable to the usual forging, rolling, or drawing processes. So remarkable was this fact, and so different from the experience at that time with metals such as copper and iron, that it has left its impress on the no-menclature within the nickel industry. To this day, furnace-cast nickel produced in such a manner as to be suitable for rolling and forging is called malleable nickel to distinguish it from the ordinary pig and shot nickel of commerce. In 1878, the firm of Jos. Wharton, of Philadelphia (which later became The American Nickel Works, a constituent of The International Nickel Co.) exhibited at the Paris Exhibition specimens of rolled pure nickel strip and of drawn nickel wire. About this time, there was considerable activity in the study of the refining of nickel and several methods were described, some of which were patented, for the production of furnace-cast malleable nickel including the use of manganese (Boed-dicker,1 Selve and Lotter2), the use of potassium permanganate (Bernsdorfer Metallwarenfabrik3) and the use of phosphorus (Garnier4). By far the most efficient method was discovered by Th. Fleitmann in 1879;5 it consisted in adding to the molten nickel, just before pouring the castings, from 0.05 to 0.125 per cent. of metallic magnesium. This soon became the recognized final malleableizing treatment for furnace-cast nickel.

Jan 1, 1925

By L. D. Anderson

WHEN, after years of troublous experiences in roasting sulfide ores with heavy dust and fume losses resulting from the equipment and methods first available, there appeared on the, scene of metallurgy that revolutionary process known as sintering, it was felt that at last there had been found the ideal method for preparing sulfide ores for blast-furnace reduction. Not only were the sulfides roasted but also the fine oxidized ores were bound together with them in strong porous cellular masses which were in the best possible condition for reduction. With the experiences gained in the manipulation of the Huntington-Heberlein, Carmichael-Bradford, and Dwight & Lloyd processes there developed a refinement of detail which brought the whole plan of roasting by sintering to a high plane of perfection. But that metallurgy is never stationary is revealed by the fact that changes in milling practice, particularly the development of flotation, have introduced a new set of problems in sintering itself. Inasmuch as it is felt that these problems have not yet been solved in an entirely satisfactory manner this paper is written to record the present practice of the Salt Lake Valley smelters with the hope that there will be brought forth such discussion as may perhaps lead to still better practice. By far the greater proportion of the sulfides smelted today are flotation concentrates. Usually they are high grade, sometimes as high as 70 per cent. and more in lead. They are extremely fine, many mills grinding the ore so that from 60 to 80 per cent. will pass through screens of 200 mesh. The physical condition in which many of these concentrates reach the smelters is disconcerting to the metallurgists. Some are of about the consistency of putty. Others are of a sticky, slimy nature. Others again, dried to the limit, are veritable powders. Remembering that the down-draft sintering charge for the best results must be porous enough to let air be drawn through it reasonably well, must be thoroughly mixed, and must have some coarse material in it to segregate out and form a layer on the grates, it will be understood that the advent of this extremely fine material has made necessary still further elaboration in the equipment and processes of preparing sulfides for the blast furnaces, all of which is expensive. The high metal contents of the concentrates

Jan 1, 1929

By Gregoire Gutzeit

The development reported in this paper was begun by the author a number of years ago, while he was a lecturer on complex chemistry and metallurgy at the University of Geneva, Switzerland, and in charge of that institution's research laboratory. Completion of the development and reduction to practice did not occur until last year at the Westport mill, laboratories and testing plant of the Dorr Company, where this method is now in general use for identifying and localizing the mineral constituents of both metallic and nonmetallic ores. It has proved to be a practical tool of the metallurgical staff at the Westport mill, devising unusual milling flowsheets for complex and refractory ore bodies. In a number of instances the findings have been successfully used as fundamental factors in the design and specification of complete metallurgical plants. Seven examples of the use of this method in solving practical milling problems are included in this paper. General Outline The microscopic study of an ore, at first only of scientific interest, has proved extremely useful both in practical geology and in ore dressing. The binocular magnifying lenses for rough observation of the products of an ore-dressing plant have been in use for a long time; but only within the last few years has a systematic microscopical examination of ore samples become a normal tool of any research laboratory dealing with ore-dressing problems. Such an investigation avoids considerable loss of time as well as empirical trials and useless experimentation. It will generally indicate the correct grinding and often will suggest the proper method of treatment. . The petrographic determination of transparent minerals in thin sections, or even in grains, has been perfected, and very accurate methods have been devised to meet any requirement, such as Feodorof's rotating stage on the petrographic microscope. Almost all transparent minerals can be positively identified by their optical properties; i.e., isotropism, anisotropism, color, pleochroism, refractory index, cleavage, crystal form, birefringence, and others. The identification of opaque minerals is a much more difficult problem and can be done only by using polished specimens. Unfortunately, most of the valuable metallic ores, and even some of the nonmetallic ones, are not transparent; therefore it has been necessary to develop a special technique for the determination of these minerals. Some optical properties—for instance, isotropism, anisotropism, color, cleavage, reflecting power-—are often adequate in roughly classifying the mineral. Only "reflecting power" is a measurable value, provided special photometric equipment (ocular photometer or Orcel's photoelectric cell) is available. The other optical properties mentioned are more or less relative,

Jan 1, 1943

By Gregoire Gutzeit

The development reported in this paper was begun by the author a number of years ago, while he was a lecturer on complex chemistry and metallurgy at the University of Geneva, Switzerland, and in charge of that institution's research laboratory. Completion of the development and reduction to practice did not occur until last year at the Westport mill, laboratories and testing plant of the Dorr Company, where this method is now in general use for identifying and localizing the mineral constituents of both metallic and nonmetallic ores. It has proved to be a practical tool of the metallurgical staff at the Westport mill, devising unusual milling flowsheets for complex and refractory ore bodies. In a number of instances the findings have been successfully used as fundamental factors in the design and specification of complete metallurgical plants. Seven examples of the use of this method in solving practical milling problems are included in this paper. General Outline The microscopic study of an ore, at first only of scientific interest, has proved extremely useful both in practical geology and in ore dressing. The binocular magnifying lenses for rough observation of the products of an ore-dressing plant have been in use for a long time; but only within the last few years has a systematic microscopical examination of ore samples become a normal tool of any research laboratory dealing with ore-dressing problems. Such an investigation avoids considerable loss of time as well as empirical trials and useless experimentation. It will generally indicate the correct grinding and often will suggest the proper method of treatment. . The petrographic determination of transparent minerals in thin sections, or even in grains, has been perfected, and very accurate methods have been devised to meet any requirement, such as Feodorof's rotating stage on the petrographic microscope. Almost all transparent minerals can be positively identified by their optical properties; i.e., isotropism, anisotropism, color, pleochroism, refractory index, cleavage, crystal form, birefringence, and others. The identification of opaque minerals is a much more difficult problem and can be done only by using polished specimens. Unfortunately, most of the valuable metallic ores, and even some of the nonmetallic ones, are not transparent; therefore it has been necessary to develop a special technique for the determination of these minerals. Some optical properties—for instance, isotropism, anisotropism, color, cleavage, reflecting power-—are often adequate in roughly classifying the mineral. Only "reflecting power" is a measurable value, provided special photometric equipment (ocular photometer or Orcel's photoelectric cell) is available. The other optical properties mentioned are more or less relative,

Jan 1, 1943

By Knut L. Sandvik, Aage Solbakken

it is an established fact that the collecting properties of xanthates and anionic collectors are dependent on the hydrocarbon chain length. This is ascribed to the greater adsorption densities caused by increasing the xanthate chain length. As batch flotation tests showed similar trends for amines, an investigation of the adsorbing properties of amines was undertaken. Because earlier investigations showed adsorption densities for dodecylamine salts on quartz varying as much as 20 times under apparently similar conditions,1-4 it was decided to make a survey of the changes in adsorption density due to the drying conditions of the quartz. EXPERIMENTAL PROCEDURE The quartz, handpicked in the pegmatite quarries of Iveland, Setesdal, had the following composition: SiO2 99.81, A12O3 0.01, Fe2O3 0.05 and loss by ig-

Jan 1, 1969

By C. H. Hitchcock

The puiblication by the Institute of a small geological map of the United States calls for an explanation of its peculiarities. The title intimates that it is intended "to illustrate the schemes of coloration and nomenclature recommended by the International Geological Congress." By way of further explanation it is said to be "based, by permission of the Director of the United States Geological Survey, upon the map published in his Fifth Annual Report, the portions not colored in that map being here supplied from other sources." The map referred to was prepared by W. J. McGee, and in the text of the report containing it he has given a list of the authorities employed in the compilation. The scheme of coloration used for the map was the one proposed by the Director, in the Seeond Annual Report, for the publications of the United States Geological Survey, which differed materially from those employed by the older American geologists. Because of the increasing diversity in the particular colors employed to represent rocks by geologists in different countries, and of the existence of very dissimilar schemes of nomenclature, it seemed best to the American Association for the Advancement of Science, at its Buffalo meeting in 1876, to appoint an international committee of geologists, who should consult together, and, if feasible, to call an International Congress to discuss these subjects. The proposition met with favor, and the meeting was called. The first session was held at Paris, in 1878, when geologists were present from twenty different countries. Once organized, the Congress has perpetuated itself, enacting regulations for its conduct, choosing the French language for its medium of communication, and arranging for the compilation of a geological map of Europe upon which the perfected schemes of coloration and nomenclature will be delineated. The American Association maintains a standing committee to represent it at the international sessions, and to report their proceedings. Sixteen countries were represented at the second Congress, at Bologna;

Jan 1, 1887

By F. R. Hensel

THE present study was rude to determine the laws governing the formation of the primary? crystal structure during solidification. Most of the experiments were carried out on chill castings, but from the results it will be possible to draw certain conclusions as far as sand cast-ings are concerned. It is necessary to discuss first a number of theories, which are generally adopted for explaining the structure of an ingot. Usually, the structure FIG. 1.-VARIOUS ZONES IN A CHILL INGOT. off an ingot consists of the following three zones (Fig. 1): (1) a chill layer of small at. random oriented crystals; (2) a layer of columnar crystals; (3) a zone of equiaxed crystals. The tensile properties of the chill layer and the equiaxed range are usually much better than in the columnar range, particularly the planes that are formed by the columnar crystals growing from two sides at right angles leave low tensile properties. This is one of the reasons why colum-nar crystals in ingot structures are undesirable.

Jan 1, 1937

By Laurence Hicks

CONSIDERATION of the past work on the subject of the diffusion of chromium into iron suggested that additional information might be given by the use of X-ray spectroscopy in following the concentration changes through the diffusion zone. Grübe and Fleischbein1 packed rods of electrolytic iron in a mixture of alumina and chromium. These specimens were heated in an atmos-phere of purified hydrogen for varying lengths of time. After treatment the specimens were examined metallographically and showed the usual structure, consisting of a border of radially oriented columnar grains ending in a sharp boundary line. Reference is made to the fact that etching with certain reagents will attack only the material inside the border of columnar growth and also to the fact that polishing seems to develop a ridge at the position of the boundary between the etched and unetched areas. By chemical analysis of thin layers turned off on a precision lathe, the authors were able to obtain depth-concentration curves. These curves, reproduced in Fig. 1, show that 'in most cases a pronounced change of slope occurs, corresponding to the position of the boundary of the columnar grains. In a later paper Grübe extends his work to other systems which show the same characteristics.2 He concludes that the reason for the break in the curve is that a hindrance of diffusion occurs at the place where the regularly oriented grains of the diffusion zone meet the random grains of the interior portion, on the assumption that the diffusion velocity in one direction in a grain may be greater than in another direction, and that the grains in the diffusion zone orient themselves so as to give the maximum diffusion rate. Kelley3 points out that Grübe has failed to note that the boundary line does not consistently cross all grains and

Jan 1, 1933

By D. O. Hobson

Zirconium single crystals of various specific orientations were fabricated by rolling or drawing. The resulting textures were determined and are discussed with respect to the deformation modes that produced them. The crystals deformed in a predictable manner by combinations of up to third-order twinning with three twinning modes and by slip. Twinning was found to play a major role in initial texture formation. Texture changes produced by slip occurred only at the higher reductions. The twinning sequences that produced each intensity peak during the initial reductions could be identified. Schmid factor criteria were found useful in predicting which deformation modes to expect for each crystal orientation and fabrication procedure. The possible application of these data to poly-crystalline material is discussed. PREFERRED orientation or texture has a significant effect on the properties of most materials, causing anisotropy in fabricated cubic metals and enhancing the natural anisotropy of noncubic metals. This study evaluates the effects of several fabrication methods on the textures formed from specific starting orientations of zirconium single crystals and, it is hoped, gives an insight into the effects of the same operations on poly-crystalline material. BACKGROUND In fcc and bcc metals, texture changes take place by gradual lattice rotations caused by the operation of one or more slip systems. Deformation twinning plays an insignificant role in the deformation of such metals. In zirconium and its alloys, however, and in many other hep metals the ability to twin allows very rapid texture changes to be made with very small amounts of deformation. The deformation systems found in zirconium and its alloys are prism slip and three twinning modes.1 Slip occurs on the {1010}< 1120) system. There is little or no appreciable basal slip in zirconium. The twinning planes, illustrated in Fig. 1, are {1012}, {ll2l}, and {1122}. Two twinning modes, the {1012} and the {ll2l} operate for a tensile stress along the basal pole. A compressive stress parallel to the basal pole is required for {ll22} twinning. These twinning operations cause a 35- to 85-deg reorientation of the basal pole. The {1012} twin is the predominant tensile twin at room temperature. The twinning shears, S, are shown in the figure. A criterion for predicting which deformation system will operate when a grain is subjected to a known stress state is the Schmid (orientation) factor. This factor gives the fraction of the applied stress that computer program was written2 to calculate the Schmid factors for the four deformation modes in zirconium. It assumed three orthogonal stress axes and considered ninety-one different orientations of the basal pole in one octant of this stress space. At each basal pole position the Schmid factors were calculated for seven positions of rotation at 10-deg increments of the unit cell about the basal pole. Schmid factors were determined for a total of 637 orientations and for twenty-four deformation systems in each orientation. The program listed the Schmid factors for uniaxial stress parallel to each axis and, to approximate rolling, or-thonormal biaxial stress was also considered. Fig. 2 shows the range of orientations over which the various types of deformation would tend to predominate in biaxial plane strain with the stresses, equal magnitude. The exact boundary position between regions of different deformation modes depends, however, on the relative values of the critical shear stress for each deformation mode. Fig. 2 is drawn on the assumption that they are equal and it therefore may be only approximately correct. It is also recognized that the biaxial stress analysis may not be applicable in certain crystal orientations. EXPERIMENTAL PROCEDURE Single crystals of zone-refined zirconium, produced by Wilson of this Laboratory,3 were electrical-discharge-machined to form specimens for rolling, tube-drawing, and rod-drawing studies. Specimens were rolled at room temperature on 2-|--in.-diam hand-powered rolls from three different starting orientations: 1) the basal plane parallel to the rolling plane and the [1120] in the rolling direction, (0001)[ll20]; 2) the (1120) plane parallel to the rolling plane and the basal pole in the rolling direction, (1120)[0001]; and 3)_the (1120) plane parallel to the rolling plane and the [1100] in the rolling direction, (1120)[ll00]. Drawing specimens were cut with the [0001] direction as the drawing direction in the tube blank and [1120] as the drawing direction in the rod specimen. The drawing

Jan 1, 1969

By R. R. Judd, H. W. Paxton

The rate of dissolution of cementite was studied in three low-carbon materials: a zone-refined Fe-C alloy, an Fe-0.5pct Mn-C alloy, and a commercial low-carbon steel. The materials were spheroidized, ad then held isothermally at temperatures above the Al. The isothermal anneal was interrupted periodically by a water quench and the specimens were analyzed by quantitative metallography for the amount of aus-tenite formed during the anneal. The results of this study were compared with an analytical model for the process, which assumes that carbon diffusion in aus-tenite is the rate-controlling step for the cementite dissolution process. The correlation between the model and the experimental data is excellent for the zone-refined Fe-C alloys; however, the Fe-0.5 pct Mn-C alloys and the commercial steel deviate from the calculated model. This deviation is thought to be a result of manganese segregation between the carbide and the matrix. The rate of nucleation of austenite at carbide interfaces was reduced by the manganese addition and enhanced by the presence of ferrite-ferrite grain boundaries. PREVIOUS investigations of the nucleation and growth of austenite from ferrite-carbide aggregates are not entirely satisfying for at least one of several reasons. The most prevalent of these is a lack of quantitative data. Engineering studies have been run on many steels with little control over important parameters such as composition and initial aggregate structure. The data obtained are valid only for material with identical chemistry and thermal history. A more informative approach to the problem of aus-tenitization would be to determine the mechanism that controls the rate of solution of carbide in austenite and how it is modified by alloying elements. This information could then be used to calculate an austeniti-zation rate for any material, provided its composition and structure are known. The object of the present work is to establish the rate-controlling step for cementite dissolution in Fe-C austenite and to investigate the modification of this rate by small manganese additions. The composition and structure of the material used were carefully controlled and all measurements were designed to allow a quantitative analysis of the kinetic process that controls the austenitization rate. A MODEL FOR DISSOLUTION OF CEMENTITE Cementite dissolution has been analyzed mathematically by a model that approximates the material used in the experiments. This model postulates a regular ar-array of identical cementite spheroids with 4 C( diam, embedded in a grain boundary- free ferrite matrix. The analysis provides a detailed description of the dissolution of one carbide spheroid and a generalization of the solution by summation over all the carbides in the material. The carbides may be isolated by defining identical, space-filling cells of ferrite around them. If the cell dimensions are greater than the diameter of the austenite sphere resulting from complete dissolution of the carbide, and no interaction (through diffusion in ferrite) takes place between cells during the dissolution process, the model need concern only one cell, since the solution in each cell is identical. In the experimental material, the dimensions of the cell, the carbide, and the final austenite sphere are approximately 24, 4, and 8 p, respectively; use of the single cell is therefore justified. The experimental observations are made on the austenite nodules that form around each carbide during the dissolution process. The model concerns the growth of these austenite nodules. The attendant shrinking of the carbide can be obtained from the same analysis by an extension of the calculations. Several a priori assumptions are necessary to make the analysis of the growth problem tractable. They are: 1) carbon diffusion through the austenite nodule is the rate-controlling process; 2) local equilibrium exists at all interfaces, 3) the austenite nucleus that forms on each carbide instantaneously envelops the carbide; 4) during the austenite growth process, the diffusion flux of carbon in ferrite is insignificant; 5) a quasi-steady state exists in the austenite concentration field; that is, at any instant during the dissolution process, the austenite carbon concentration gradient closely approximates that for a steady-state solution; and 6) the effects of capillarity on the dissolution rate of the carbides can be neglected. Referring to Fig. 1, a mass balance at the y-a interface for an infinitesimal boundary movement gives: Where rb is the outer radius of the austenite shell, C1 and C are carbon concentrations at the interface in austenite and ferrite, respectively, see Fig. 2, is the diffusion coefficient of carbon in austenite for the concentration of carbon at the interface, and t is time. The fifth assumption permits the austenite carbon concentration to be approximated by the Laplace solution for the spherical case. Therefore, where C(Y) is the carbon concentration at r, and A and B are constants. Local interfacial equilibrium fixes the boundary conditions for the diffusion problem. They are:

Jan 1, 1969