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By M. G. Benz

The superconducting performmce of diffusion-processed Nb3Sn is influenced by its micro structure. High isotropic transverse current density may be achieved in this material by a process which forms a precipitate of ZrO, within the Nb3Sn. FOR an ideal type-I1 superconductor, little or no transport current can be carried in the mixed state; i.e., little or no transport current can be carried above the lower critical field H,,, where the field penetrates abruptly in the form of current vortices or fluxoids, even though full transition to the normal state does not occur until the upper critical field H,,.' Fortunately, nonideal type-I1 superconductors can be readily obtained and these carry large transport currents up to the upper critical field H. Both theoretical and experimental investigations have attributed this current-carrying capability for nonideal type-I1 superconductors to pinning of the fluxoid lattice by heterogeneities in the microstructure of the superconducting material. These heterogeneities may take the form of dislocations or dislocation clusters,2"5 grain boundaries: structural imperfections introduced by phase transformations; radiation damage,8"10 or precipitates.11"15 Nb3Sn formed by diffusion processing is a type-I1 superconductor. Heterogeneities are needed for high superconducting critical currents above H,,. This paper will cover: a) what the microstructure of diffusion-processed NbSn looks like; b) what changes in the microstructure take place when the system is doped with precipitates, and c) how these changes in microstructure influence the superconducting critical currents. EXPERIMENTAL Preparation of Samples. Diffusion processing was used to form the Nb3Sn. The procedure used was as follows: a) coat the surface of a niobium tape with tin; b) heat-treat this tape at a temperature above 930°C to form a layer of Nb3Sn at the Sn-Nb interface. Such a layer of NbsSn is shown in Fig. 1 The thickness of the NbsSn layer formed was controlled by the time and temperature of the heat treatment. The same general procedure was used for preparation of both undoped samples and samples doped with a precipitate. An additional step was included in the preparation of the doped samples which consisted of internal oxidation of zirconium to form ZrOn. The details of the doping process will be reported in a later paper. Sample Testing. The Nb3Sn tape samples were soldered to a copper or brass shunt. Current and voltage leads were then attached to the sample in the usual four-probe resistance measurement configuration. The sample was cooled to 42°K. In some cases it was cooled in the presence of a high magnetic field and in other cases with the field turned off. The results were the same for both cases. The samples were oriented in a configuration with field transverse to current but could be rotated such that the angle between the field vector and the wide side of the tape sample could be changed. Measurements up to 100 kG were done in a superconducting solenoid and measurements above 100 kG in a water-cooled copper magnet at the MIT National Magnet Laboratory. Once the test field was reached, the current in the sample was increased until voltage was detected across the sample. The critical current was taken as the current at which voltage was first detected in excess of background noise. In most cases this was 1 to 2 x 10~6 v for a— in.-wide sample carrying several hundred amperes with a in. separation between voltage leads and with a 10 "-ohm shunt resistance. RESULTS AND DISCUSSION Microstructure. Examination of the microstructure of the undoped Nb3Sn shows rather large-diameter (1 to 2 columnar grains growing outward from the niobium surface toward the tin surface. As the layer is made thicker by longer diffusion times, these grains grow longer. Few new grains are started. Transmission electron microscopy shows little or no second-phase material within the bulk of the Nb3Sn layer. The microstructure of a diffusion-processed NbsSn layer changes quite drastically when the system is doped so as to form a precipitate within the NbsSn layer. Instead of large-diameter columnar grains of NbaSn forming, smaller-diameter (0.5 to 1 ) equiaxed grains of Nb3Sn decorated with the precipitate form. Fig. 2 shows a transmission electron micrograph of a Nb3Sn layer doped with zirconium oxide. This layer has been etched so that one may look between the grains

Jan 1, 1969

By E. W. Johnson, M. L. Hill

Cold working of iron-carbon alloys was found to increase greatly the hydrogen solubility and to decrease the diffusivity at temperatures up to 400° C. These effects are increasing functions of both the carbon content and the degree of deformation. The hydrogen behavior is consistent with the idea that cotd working creates "traps", which are concluded to be microcracks in which the hydrogen is chemisorbed. Hydrogen embrittlement is explained by the Petch theory of metal crack surface energy loss due to hydrogen adsorption. HYDROGEN embrittlement of steel has been studied for many years and has been the subject of an extensive literature, but the mechanism of the effect has not been completely understood. The embrittlement is unusual in that the ductility loss is not accompanied by an increase of the yield strength, being primarily a decrease of the fracture strength alone. The loss of fracture strength is usually most severe in the temperature range between 0°and 100°C. Here the solubility of hydrogen in the iron lattice at ordinary H2 pressures is extremely low while the diffusivity is still quite high. From the relationships between the ductility and the hydrogen content, test temperature and strain rate, it is apparent that the hydrogen atoms causing the ductility loss difbse to and concentrate in small regions of the metal which are especially susceptible to the initiation and propagation of fracture. This hydrogen segregation apparently occurs after plastic straining has begun. Below 0°C the ductility loss persists only at low strain rates in confirmation of the view that the embrittlement is diffusion .controlled. The tendency of the embrittlement to disappear above 100°C can be explained by the increasing lattice solubility of hydrogen with rising temperature. A common view of hydrogen embrittlement of steel is that the hydrogen initially dissolved in the metal lattice diffuses to structural discontinuities and there precipitates as H2 gas at very high pressures which assist the external stress in causing premature failure.1,2 The idea of a high H2 pressure in equilibrium with ordinary amounts of hydrogen in steel at room temperature is due to observations of hydrogen behavior in fully annealed material, for which the Sieverts' law constant relating solute concentration to H2 pressure is extremely small. Hydrogen-embrittled steel, however, is always plastically deformed to some extent, and therefore it is important that hydrogen embrittlement be explained primarily in terms of hydrogen behavior in plastically deformed material. Such an explanation is attempted in this paper. Previous studies of hydrogen in cold-worked steel have shown that both the solubility and the diffusion rate are significantly chaned when the steel is cold worked. Darken and Smith discovered that the amount of hydrogen absorbed from acid by cold-rolled steel at 35°C is many times greater than that absorbed by hot-rolled steel. They found also that the hydrogen permeability of the steel is unaffected by cold working. Keeler and Davis4 confirmed the high apparent solubility of hydrogen in cold-worked iron-carbon alloys at temperatures up to and even beyond the recrystallization temperature. They also found that this solubility increase accompanying cold work is a sensitive function of the carbon content, being absent when no carbon is present. The present experimental study was undertaken primarily to obtain an improved understanding of the behavior of hydrogen in cold-worked steel. Data were obtained on the effects of temperature, H, pressure, carbon content, and degree of cold work on the hydrogen solubility and diffusivity in iron-carbon alloys. These data have been helpful in elucidating the nature of the cold-worked steel structure as well as in providing information on the mechanism of hydrogen embrittlement of steel. EXPERIMENTAL Cylindrical specimens for hydrogen absorption and diffusion rate measurements were prepared from three iron-carbon binary alloys and a commercial SAE 1010 steel. The iron-carbon alloys were prepared by vacuum melting electrolytic iron with graphite in a magnesia crucible. The alloys were cast in vacuum as 2 1/2-in. sq ingots weighing about 20 lb each. The ingots were hot rolled (above 1900°F) to 5/8-in.-diam round bars and then cooled in air to room temperature. The resulting metallographic structure consisted of islands of fine pearlite surrounded by free ferrite. Chemical analyses of the materials are given in Table I. The 5/8-in. diam bars were turned to diameters such that cold reduction to the desired final specimen diameters would result in either 30 or 60 pct reduction in area (RA). The machined bars were then cold worked by swaging at room temperature

Jan 1, 1960

By M. Rudolph, E. Schach, M. Buchmann, T. Leißner, N. Krupko, U. Peuker, M. Kern

"In mineral processing, density and magnetic susceptibility are two very fundamental properties. For the beneficiation of valuables to produce a saleable concentrate a detailed understanding of these properties is essential. Especially when it comes to the processing of cassiterite, which is the main mineral for tin production, they become highly prominent. Due to the chemically inert character of cassiterite towards most industrial applied leaching agents, density and magnetic separation processes are mainly applied for its beneficiation. To guarantee an optimized utilization of the different operations not only cassiterite but also the different gangue minerals have to be considered. In this study, a skarn ore is characterized by density and magnetic susceptibility. Therefore, the material was first split into different density classes by heavy liquid separation. The obtained classes were further separated by their susceptibility to finally obtain a density-susceptibility matrix. For this purpose, an isodynamic separator was used. A more detailed characterization of the materials is done via gas pycnometer, magnetic susceptibility balance and vibrating sample magnetometer to estimate the characteristics of density and susceptibility for the various classes. Further, the determination of the chemical assay and the mineral intergrowth by mineral liberation analysis is used to generate a three dimensional database for detailed characterization of the present ore. The objective of this study is to estimate potential material streams for a modular processing plant via characterization of the material for the entire deposit by the two afore mentioned characteristic properties. The established multidimensional data matrix, enables predictions for the separation properties of the material and contributes to the characterization of the deposit within the context of geometallurgy."

Jan 1, 2018

By James A. Lewis

It is the purpose of this paper to show the importance of sand characteristics, when combined with other physical data, in evaluating production obtained by secondary recovery operations, and to indicate the benefits to be gained from the application of these principles to primary production. Introduction During the past 10 years there has been a growing interest within the industry regarding the movement of fluids through oil reservoirs. A number of research projects have been directed toward the development of the physical laws governing this movement. In the period 1933 to the present, correlations between laboratory analysis of cores, reservoir fluids and well performance have been established and have been applied to successful secondary water-flooding recovery operations; and to the completion, production, reconditioning and evaluation of wells in new fields. The application of these data to water-flooding, either natural or artificial, is comparatively new, but the principlcs involved were set forth in 1880 by John F. Carll,1 who said: The flooding of an oil district is generally viewed as a great calamity, yet it may be questioned whether a larger amount of oil cannot be drawn from the rocks in that way than by any other, for it is certain that all the oil can-not be drawn from the reservoir without admission of something to take its place. If one company owned all of the wells drawing upon a pool, and had accurate records of the depth and characteristics of the oil producing stratum in each well, it is quite possible that some system might be devised by which water could be let down through certain shafts, and thus the rocks be completely voided of oil and left full of water. As it is, however, no systematized plan of action can be adopted. The careless handling of one well. by which water is let down to the oil rock, may spoil several others belonging to different parties. A clashing of interests at once arises and is likely to result in disaster to the whole district. In judging of the probable effects of the intro-duction of water into any particular oil district several things are to be considered. (1st) The time of flooding—whether early in the progress of development, while yet a large percentage of oil remains unexhausted or at a later period after the supply has suffered from long continued depletion. (2nd) The structure of the rock—whether regular and homogeneous throughout, or composed of fine sand inter. bedding connected and irregular layers of gravel, sometimes lying near the top and at others near the bottom. (3rd) The shape of the area being flooded. (4th) The position of the point at which water is admitted. in relation to the location of the surrounding wells still pumping oil. (5th) The height (which governs the pressure) of the column of water obtaining admittance. (6th) The duration of the water supply. Although we may take exception to part of Carll's reasoning, particularly " and thus the rocks be completely voided of oil and left full of water," we must give him credit for pointing out the increased effectiveness of water encroachment in displacing oil from a sand and for his recording six of the present seven considerations necessary for evaluation of production of oil by water

Jan 1, 1942

By G. R. Fitterer

Trends in slag composition in acid open hearth practice, particularly the variation in iron and manganese oxides during refining, are reviewed. A procedure which is currently being used to control the refining reactions is described and partially explained through slag phase diagram considerations. In addition, the ionic nature of these slags is considered and it is proposed that silica combines with the oxide ion and forms a series of complex silicate ions. The effect of basic oxides such as FeO, MnO, and CaO is apparently additive in furnishing the oxide ion for this purpose. IT is now possible to control192 the refining of steel in an acid open hearth furnace to a surprising degree. This control has been brought about through the knowledge and use of several facts and tests. These are: 1—A planned charge analysis based on a knowledge of the type of fuel, the bath depth, etc. 2—Knowledge and control of rate of fuel input as well as its method of atomization, if any. 3—Determination of the slag fluidity. 4—Bath temperatures (use of the Pt-Pt-Rh thermocouple). 5—Periodic determination of carbon content (use of the Carb-analyzer or Carbometer). Through the use of these control methods, a heat may be made to "melt-in" with or without residual manganese and silicon. The rate of refining or carbon elimination may be controlled accurately, and the desired tapping (or "go-ahead") carbon may be approached at a rapid or slow rate according to preference and type of steel being made. Thus operating time may be predetermined and greatly reduced. Further, all of the refining can be done without any ore or other oxidizing additions, and the heat may be brought to the desired tapping temperature simultaneously with the attainment of the desired carbon analysis. This control procedure is being used in most acid plants in the United States today and has been de- scribed.', ' Although the slag metal relations are sufficiently well known to control the heat as stated, yet it is possible to account for only about two-thirds' of the 0, which must have been used for the elimination of the carbon and other metalloids. Phase diagram studies' of the slags, slag weights, the metal particle theory,' ore additions, limestone additions, etc., may all be taken into consideration; yet, the mechanism of oxidation and source of all the oxygen remain to be explained. This paper reviews some of the principles upon which the control methods were based and proposes other possibilities regarding the unexplained phenomena. Old and New Acid Open Hearth Practice Some of the recent statements in the literature regarding acid open hearth operation are based on old heat data which are not typical of modern American practice. These old heat logs have been responsible for many misconceptions regarding the acid hearth practice and represent heats which do not coincide with modern methods. In recent years, American practice has been altered materially and these changes will be briefly described. Modern American Practice: A typical log of a modern American acid open hearth heat' is shown in Fig. 1 which indicates that the refining time was only two hours, during which the carbon was eliminated rapidly and the bath temperature increased at a fast rate. The manganese and silicon contents of the metal were essentially eliminated and their oxides had become constituent parts of the slag at the "melt-down" period. During the course of the heat, the MnO content of the slag remained practi-

Jan 1, 1954

By A. McKenzie

During the late 1990s Anglo American PLC was evaluating the Gamsberg zinc deposit in the Northern Cape Province. As the primary South African metallurgical technology provider, Mintek became involved in the evaluation of a pyrometallurgical process for the recovery of zinc from the Gamsberg deposit. eloping DC arc furnace technology for the metallurgical industry. This includes the patented Enviroplas® process for the treatment of zinc bearing waste materials. As a consequence Mintek has developed extensive expertise in the pyrometallurgical processing of zinc bearing materials. However, Mintek?s technologies stopped with the production of Prime Western Grade (PWG) zinc. Early on in the evaluation of the Gamsberg project, it became evident that the refining of PWG zinc would play an important part in the economic viability of the project. At the time the only pyrometallurgical technology available for the refining of PWG zinc to Special High Grade (SHG) zinc was the New Jersey process. This process represents 50-year-old technology and has not undergone significant refinement since the technology was developed. In order to provide a complete pyrometallurgical flow sheet for possible implementation at Gamsberg, Mintek assessed the New Jersey process with a view to either improving the technology or developing a new technology appropriate to the 21 century. In 1998 Mintek convened a consortium consisting of Mintek, the University of Cape Town, Eskom Enterprises, Bateman Metals and Anglo American PLC. The consortium successfully applied to the Innovation Fund for funding to develop a new process for the pyrometallurgical refining of PWG zinc to SHG zinc. The main aims of the project were to develop a new technology for pyrometallurgical zinc refining that conformed to the following: ?Decrease the production cost of SHG zinc metal to stimulate the development of the Gamsberg deposit. ?Be compatible with the current Enviroplas® process, preferably as an add-on to that process. ?Should use electrical energy to benefit from local price tariffs. The project commenced at the beginning of 2000 and consisted of three phases: ?an initial technology search and assessment of the fundamental aspects of zinc distillation. ?the design of a pilot plant for zinc refining. ?the manufacture, commissioning and operation of the pilot plant. A new technology based on a DC arc boiler feeding a packed distillation column was developed and during 2003 the project culminated in the successful operation of a 200 kg/h pilot plant. Ultimately, all of the aims of the project were met and the main outcome is that an advanced process for the pyrometallurgical refining of zinc (the Zincref process) has been developed. The main innovation of the technology was the switch from an energy transfer limited process to a mass transfer limited process (for which a patent has been registered).

Jan 1, 2004

By A. J. Opinsky

ThE superior performance of nonsag tungsten wire in lamps has been ascribed to the large-grained micro-structure that can be developed in it. The orientations of these large grains have been studied several times; most published data1-' appear to be similar to those plotted in Fig. 1. These new data were obtained by X-ray back-reflection Laue technique from all of the large grains occurring in thirteen different wires that had been heated at the lowest possible temperature for the formation of large grains. Here the wire axis is plotted in terms of the principal directions of the cube. Rosi decided that the preferred orientation of the large crystals could be described by a single ideal orientation, (531), being parallel to the wire axis.' Rieck2,3 and Mannerkoski' have essentially confirmed this finding. Opinsky, Orehotsky, and Seigle argued that the data suggest that (211) is parallel to the wire axis instead of a single ideal orientation.5 This {211} contains the (531) ideal orientation and would appear to be a more general case. Ahlborn and Wassermann report that their orientation data stretch from ( 110) through (531) to (311) 8 This is part of the locus of (211). All these investigators have determined the orientations of the large grains by back-reflection Laue techniques. They have all obtained essentially similar results. On the other hand, Swalin and Geisler, who obtained their data by neutron diffraction, indicated that the preferred orientation of the large grains in doped wire is (110) .7 These findings cannot presently be reconciled with the pole density data described in the previous paragraph. Rosi1 and Rieck2 have advanced arguments about how their orientations could occur. Nevertheless, the crystallographic link between the (110) (cold-worked) fiber texture and the preferred orientation of the large grains has remained missing. This link can be provided through the concept of coincidence-type boundaries. Such boundaries separate two grains that have a certain number of common lattice sites. Coincidence relationships that result from rotations about low index directions are given by Brandon et a1 .' What is desired is a calculation of those orientations that bear a coincidence relationship with the (110) fibers of the cold-worked matrix. This situation arises in the following fashion. Heating the tungsten wire for a combination of time and temperature falling short of the formation of the nonsag structure yields a structure that is still fibrous in nature and the preferred orientation remains (110). During grain growth, the growing grain is in contact with these fibers. It is hence possible that the entire process may begin by the passage of a coincidence boundary into a (110) fiber. The calculations were carried out analytically and checked graphically. Following Brandon et a1.,8 coincidence relationships from 1 in 5 to 1 in 19 have been considered. The results of the calculations are given in Fig. 2. Of the coincidences examined, some of those occurring upon rotation about ( 110) come closest to the experimental points in Fig. 1. Nineteen of the twenty-three data points in Fig. 1 can be attributed to the ideal orientations A, B, C, and D in Fig. 2. As determined analytically, three crystals lie within 4 deg of point A, four lie within 21/2 deg of point B, eleven lie within 5 deg of point C, and one lies within 1 deg of point D-a total of nineteen. The off-lying points are near the |110| point of the triangle.

Jan 1, 1968

By James A. Lewis

It is the purpose of this paper to show the importance of sand characteristics, when combined with other physical data, in evaluating production obtained by secondary recovery operations, and to indicate the benefits to be gained from the application of these principles to primary production. Introduction During the past 10 years there has been a growing interest within the industry regarding the movement of fluids through oil reservoirs. A number of research projects have been directed toward the development of the physical laws governing this movement. In the period 1933 to the present, correlations between laboratory analysis of cores, reservoir fluids and well performance have been established and have been applied to successful secondary water-flooding recovery operations; and to the completion, production, reconditioning and evaluation of wells in new fields. The application of these data to water-flooding, either natural or artificial, is comparatively new, but the principlcs involved were set forth in 1880 by John F. Carll,1 who said: The flooding of an oil district is generally viewed as a great calamity, yet it may be questioned whether a larger amount of oil cannot be drawn from the rocks in that way than by any other, for it is certain that all the oil can-not be drawn from the reservoir without admission of something to take its place. If one company owned all of the wells drawing upon a pool, and had accurate records of the depth and characteristics of the oil producing stratum in each well, it is quite possible that some system might be devised by which water could be let down through certain shafts, and thus the rocks be completely voided of oil and left full of water. As it is, however, no systematized plan of action can be adopted. The careless handling of one well. by which water is let down to the oil rock, may spoil several others belonging to different parties. A clashing of interests at once arises and is likely to result in disaster to the whole district. In judging of the probable effects of the intro-duction of water into any particular oil district several things are to be considered. (1st) The time of flooding—whether early in the progress of development, while yet a large percentage of oil remains unexhausted or at a later period after the supply has suffered from long continued depletion. (2nd) The structure of the rock—whether regular and homogeneous throughout, or composed of fine sand inter. bedding connected and irregular layers of gravel, sometimes lying near the top and at others near the bottom. (3rd) The shape of the area being flooded. (4th) The position of the point at which water is admitted. in relation to the location of the surrounding wells still pumping oil. (5th) The height (which governs the pressure) of the column of water obtaining admittance. (6th) The duration of the water supply. Although we may take exception to part of Carll's reasoning, particularly " and thus the rocks be completely voided of oil and left full of water," we must give him credit for pointing out the increased effectiveness of water encroachment in displacing oil from a sand and for his recording six of the present seven considerations necessary for evaluation of production of oil by water

Jan 1, 1942

By Daniel K. Kim

The charge for the copper refinery is a mixture of anodes produced at San Manuel from BHP source concentrate and copper purchased from external sources. Control of unwanted impurities in the tankhouse - is very important and beneficial. Currently available removal/recovery technologies were reviewed for the control of bismuth and antimony levels in the electrolyte. Recent studies have focused on solvent extraction (SX) technology and generated successful results for the removal and subsequent recovery of bismuth and antimony. The SX system employs the reagent, ACORGA SBX-50, in conjunction with a patented high chloride stripping system. The latter enables recycle of the eluant, avoiding the high costs associated with conventional systems, such as regeneration of resin. Concerns over potential transfer of organics and chloride ion to the electrolyte were readily addressed, solved and demonstrated using conventional, established technology. This paper describes the benefits of electrolyte purification, the flexibility afforded by the SX system, the operational practices necessary for maintaining adequate control of bismuth and antimony impurities in the electrorefining environment and possibilities for future development /exploitation of the Zeneca SX system at the San Manuel refinery.

Jan 1, 1998

By Masaomi Kurihara, Seiya Kawano, Norihiro Yamaji, Satoshi Shiokawa, Nobuyuki Okamoto, Hironobu Sakurai

Seafloor polymetallic sulphides are distributed in the EEZ of Japan, including substantial deposits in the Okinawa Trough and Izu-Bonin back-arc basin. In this new frontier, the successful development of these resources in Japan is expected to bring about a new domestic supply of mineral resources. The initial stages of this development are authorized by the Basic Plan on Ocean Policy, approved by the Japanese Cabinet on April 26, 2013, and the Plan for the Development of Marine Energy and Mineral Resources, formulated by the Ministry of Economy, Trade and Industry (METI) on December 24, 2013. In 2008, the Japan Oil, Gas and Metals National Corporation (JOGMEC), commissioned by METI, began a survey and technological development programme for the development of the seafloor polymetallc sulphides (PMS) based on these Plans. The examination of four different fields: the evaluation of the amount of the resource, environmental assessment, mining technology, and processing & smelting technology, are concurrently promoted, aiming for commercialization as soon as possible. Based on the results of research for properties of geomorphology and marine environments of the target test sites in the Okinawa trough, which have been ongoing for several years, the preparation of the pilot lifting test included an in-situ excavation and crushing test conducted using test excavating and crushing systems.

Jan 1, 2018

By E. J. Harvey

The Ozarks has been called "a diamond in the rough". In this region streams have steep gradients, sparkling clear flows of cold water fed by many springs, and a wildness that is almost unique in the central part of the United States today. The Current River and its tributary, Jacks Fork, have been set aside for preservation by the National Park Service as a "Wild River" in the first park of its kind in the country. It is called the Ozark National Scenic Riverway. Similarly, responsibility for the preservation of the Eleven Point River has been assigned to the U. S. Forest Service. Protection of other streams in the Ozarks has been considered by State agencies. The hydrologic system of the Ozarks is a complex network of gaining and losing streams, caves, conduits, and large springs. Increased sewage loads derived from the growing towns and expanding tourist trade are a potential hazard; effluents may flow underground for long distances, polluting springs and wells. To add another dimension to the hydrologic picture a new lead industry is also flourishing in the Ozarks. Although the history of lead mining in the area goes back to 1701 (U. S. G. S., p. 43), the area has not seen a revitalization like the one that has been developing in the last 10 years; and the economic growth promises to continue indefinitely. Although this brings capital expenditures and wages into the area, it also brings potential hydrologic problems. Chemicals, wastes and other substances either stored on the surface or transported across it are subject to accidental spillage. In an area where these substances remain on the surface their effects are subject to surveillance. In the Ozarks, however, this may not be possible.

Jan 1, 1970

By Oliver C. Ralston

The Nonmetallic Minerals Division of the Bureau of Mines deals with all mineral substances not intended to be used as ores for extraction of metals, with the exception of the fuels. However, coal washing, the methods of which are highly Similar to the concentrating methods for ores, is included In the work of the Nonmetallic Minerals Division to facilitate administration and to avoid duplication of equipment. During the fiscal year most of the work of the division was done at the experiment stations in College Park, Md. Tuscaloosa, Ala., and Seattle, Wash.

Jan 1, 1938

By H. O. Hofman

Lime-roasting is a term proposed by Ingalls' for the operation of forcing air under pressure through a mixture of galena and lime at the kindling-temperature with the object of oxidizing lead and sulphur and of fritting or fusing the charge. If finely-divided galena were treated in this manner without the addition of lime, the heat set free by the oxidation of part of the lead and the sulphur would be sufficiently great to fuse un-decomposed sulphide, and thus stop desulphurization. Besides the chemical action that the addition of lime, limestone or gypsum to the charge may have, the admixture has the physical effect that it keeps the particles of galena separated from one another and accessible to the oxidizing effect of the air. At present, three methods of lime-roasting are carried out on a working-scale,—the Huntington-Heberlein, the Carmichael-Bradford and the Savelsberg2 processes. In the last, which interests us here, an 8-ton charge is made up of galena, limestone and perhaps some siliceous or ferruginous flux; the whole is crushed to pass a screen with 3-mm. holes and moistened with 5 per cent. of water. It is fed gradually into a bowl-shaped converter, 6.56 ft. in diameter, supported by trunnions attached to a truck. On the bottom the converter has a grate with blast-inlet beneath. In starting, the truck with the converter

Jan 1, 1908

By Alexander Field

THE rate of elimination of carbon largely controls the time required to make a heat of steel by the basic open-hearth process and to an important degree determines the cost of refining. Practical experience has led to the generally accepted belief that the use of slags relatively high in iron oxide, such as are required to bring about rapid refining, leads to a certain sacrifice of quality in the product. As a consequence, a compromise must be made between the exceedingly slow rate of carbon drop which would correspond to the ideal case and the rapid rate which would best satisfy the condition of minimum cost. An increase in rate of refining necessarily implies an increase in the concentration of iron oxide dissolved in the metal. However, even for the infinitely slow rate that corresponds to slag-metal equilibrium, the metal would contain a certain definite concentration of dissolved iron oxide. It is a matter of great practical importance, therefore, to determine the quantitative relation between the minimum or equilibrium concentration of iron oxide in the metal and the higher concentrations which must actually obtain in practice. The present paper is devoted to the development of certain equations, derived from the established laws of physical chemistry, which will enable this relation between rate of refining and the degree of oxidation of the metal bath to be computed from operating data. No attempt is made to exhaust the possibilities of this general method of treatment. In considering rate of refining, attention is mainly confined to rate of carbon elimination. However, the equations are of a more general nature and their application may readily be extended. The results of the preliminary calculations given herein indicate that increased rate of refining may have a decided effect in increasing the concentration of iron oxide dissolved in the metal. The uncertainty. which attaches to the calculated value for this relationship arises in part from probable errors in experimental data on which the calculations are based, and in part from the lack of complete or favorably disposed information on basic open-hearth practice.

Jan 1, 1928

By R. M. S. Häggblad

The article deals with stabilisation and regeneration of Ce02 and Ce02/Zr02 based Pt water gas shift catalysts, subject to high initial deactivation. The reaction gas species effect on the catalyst deactivation was investigated by H2-TPR. Activity measurements enabled the effect of different promoters, some added to the Ce02 based catalysts and some to the Ce02/Zr02 based Pt catalysts, to be investigated. The catalysts were also characterised by BET and CO-TPR. Deactivated catalysts activity was restored by using various regeneration methods. Of the two selected carriers the Ce02/Zr02 based Pt catalyst showed the highest resilience to deactivation. For the two different carriers, Ce02 and Ce02/Zr02, Wand Re were the best promoters when the catalyst was subject to deactivation. Experiments with Hr TPR indicate a fast initial change in the platinum oxides concentration and composition. The CO-TPR was used to make conclusions about the various regeneration effects of water and oxygen on the catalyst. Finally it is suggested that not one deactivation mechanism is possible and which mechanism that dominates is dependant on the catalyst and the reaction gas composition.

Jan 1, 2005

By E. Miller, J. M. Eldridge, K. L. Komarek

Aclivilies of magnesium in liquid Alg-Si alloys have been delermined between 5 and 60 at. pcl Si, close to the melling point of Mg2Si, by an improved isopieslic melhod. Silicon specinrens, held in alumina crucibles and graplrile conlainevs of special design, were healed in a letrlpevalure gvadient and equilibrated with mag-nesilcrrl rapor in a closed lilanium system. The ther-madynamic Junctions were calculated and compared with the thermodyuamic properties of the other three mg- Gvoup IVB systems. Lattice paramelers of three Mg2X compounds were measured. The bonding in the Mg2X compounds is largely covalent with small and uarying amounts of metallic and ionic conlvibutions. The Mg-Si phase diagram1 has one congruent melting compound, Mg2Si, of essentially stoichiometric composition, two eutectics, and very limited terminal solid solubilities. Little information is available on the thermodynamic properties of this system. The free energy of formation of Mg2Si has been determined by the Knudsen cell technique2 in the range 572" to 680oC, by the transportation method3 between 858" and 950oC, and by the electromotive-force method4 in the range 400o to 600°C. Kubaschewski and villa5 and caulfield6 have measured the heat of formation of Mg2Si. An electromotive-force study of magnesium-rich liquid alloys was recently published by Sryvalin el al.7 The present investigation was undertaken to complete a general survey of the thermodynamic properties of the homologous series of Mg-Group IVB systems, i.e., Mg-Pb,a9,Mg-Sn,10,11 mg-Ge,12and Mg-Si. An isopiestic technique, previously developed for similar measurements on liquid Mg-sn11 and Mg-Ge alloys,12 was modified for the Mg-Si system. Specimens of the nonvolatile component, silicon, were contained in dense alumina crucibles placed inside covered graphite crucibles which were heated in a temperature gradient in an evacuated and sealed titanium reaction tube and equilibrated with magnesium vapor of known vapor pressure. The alumina crucibles prevented contact between the highly corrosive liquid Mg-Si alloys and graphite. The graphite cruci- bles effectively preserved the high-temperature equilibrium composition of the liquid alloys containing highly volatile magnesium on termination of the experiments during the quench to room temperature. EXPERIMENTAL PROCEDURE Silicon of semiconductor-grade purity (E. I. du Pont de Nemours and Co., Brevard, N.C.) and 99.99+ pct Mg (Dominion Magnesium Ltd., Toronto, Canada) were used. Graphite crucibles with press-fitted lids were machined from high-density (1.92 g per cu cm) rods (Basic Carbon Corp., Sanborn, N.Y.) which had a maximum ash content of less than 0.04 pct. The alumina crucibles had a purity of 99.7+ pct (Triangle RR grade, Morganite, Inc., Long Island City, N.Y.). In preliminary runs the liquid alloys were contained in graphite crucibles following the exact procedure developed for the Mg-Ge system.'2 These runs failed due to appreciable reaction between the molten Mg-Si alloys and graphite, and the results have been discarded. The procedure was then modified and the Mg-Si alloys were subsequently held in alumina crucibles. For most of the runs alumina crucibles of known weight and approximately 6.3 mm ID, 12.5 mm height, 1.0 mm wall thickness were loaded with weighed amounts of silicon and encapsuled in tightly covered weighed graphite crucibles 5/16 in. ID, 2 in. helght, 3/32 in. wall thickness). The graphite crucibles were machined from rods which were 85 pct of the theoretical density. These crucibles were therefore sufficiently porous so as to permit magnesium vapor to effuse through the silicon under the experimental conditions of approximately 970O to 1220°C and 1 day equilibration time. However, negligible magnesium was lost from the crucible during the quench due to the slow effusion rate through the pores of the graphite. The inner alumina crucible prevented the liquid alloys from contacting the graphite, and the very tightly fitting graphite crucible lids served to retain any magnesium vaporizing from the alloys inside the crucibles during the quenching step.12 The loaded silicon-alumina-graphite cells were positioned, one above another, on a 16-in.-long titanium thermocouple well and tied securely to the titanium tube with thin molybdenum wires held in grooves around the circumference of the graphite crucibles. A thin (0.005-in.) molybdenum strip prevented contact between the graphite crucibles and the titanium. This assembly was lowered into a titanium reaction tube (la in. ID, 16 in. long, $ in. wall thickness) closed on one end which contained a 11/2-in.-long cylinder of magnesium at the bottom. The inner titanium thermocouple well was positioned eccentrically in the large tube because of the eccentric mounting of the cells on the well. Appropriate modifications of the titanium cap"'12 were made to join the inner and outer titanium

Jan 1, 1968

By A. E. Jenkins, O. C. Roberts, D. G. C. Robertson

Using an inverted-cone coil at 450 kHz, it has been possible to levitate iron (FeS), cobalt (CoS), and nickel (NiS) sulfides. Important nontransition metal sulfides such as ZnS, PbS, and Cu2S have proven impossible to levitate although Cu-Fe-S ternary alloys containing 30 wt pct S and up to 10 wt pct Cu, and Cu-Co-S and Cu-Ni-S ternary alloys containing 30 wt pct Cu have been levitated. The levitation technique has been used in preliminary experiments on the vaporization from liquid sulfides and the reaction of liquid metal-sulfur alloys with oxidizing atmospheres. The course of the reactions with pure oxygen were followed using highspeed photography and two-color pyrometry. ELECTROMAGNETIC levitation is now established as a basic laboratory technique in high-temperature research but its application has been restricted mainly to metals and alloys. Applications have included alloy preparation,' metal purification,2'3 determination of liquid metal densities and emissivities,4,5 and studies of metal supercooling,4 alloy thermodynamics,6 and vaporization phenomena.7-9 The application of the technique to compounds has not been considered previously. The successful investigation of the reactions between dilute iron alloys and oxidizing atmospheres10'1 has prompted the current physico-chemical studies involving levitated metal sulfide drops and flowing inert or oxidizing atmospheres. This paper presents the results of such a study and provides a basis for future studies involving a wide range of other compounds of metallurgical interest. The successful levitation of many metal sulfides and mattes provides a method of studying the oxidation reactions fundamental to flash-smelting and similar pyrometallurgi-cal operations under closely controlled laboratory conditions. In addition the system allows the use of a controlled atmosphere (e.g., a gas stream of a certain H2/H2S ratio) with a particular chemical potential to study the relevant thermodynamic equilibria or the mass transfer processes between the atmosphere and the levitated drop under conditions where the hydrodynamics of the system can be closely defined. The optimum frequency for the levitation melting of metals in an inverted-cone coil type inductor is within the radio frequency range 400 to 500 kHz. At frequencies lower than 10 kHz the rate of heat generation is usually insufficient to melt the levitated charge' or where melting is achieved, "dripping" from the charge is encountered.'' At frequencies above 2 mHz the levitation force decreases. Metals, alloys and preheated elemental semiconductors such as germanium and silicon, have been levitated but the levitation of only a few metal compounds has been reported. Jostsons13 and the authors have levitated liquid titanium-oxygen alloys containing 50 at. pct 0 while clark14 has reported the levitation of mixtures of FeS and MnS for short periods. With a "cold crucible" inductor sterling15 has melted ferrites by preheating them by induction in a 4 mHz field and melting at a lower frequency. However this second type of inductor has been designed purely for the melting of materials without contamination; there is only a small gas film between the charge and the inductor and the electromagnetic levitation effect is of secondary importance. For this reason further discussion will be restricted to the use of the coil type inductor. The assessment of the suitability of a particular metal compound for levitation is based upon the following two criteria: i) thermal stability, and ii) physical "levitability". In this paper these two criteria will be considered separately. The thermal stability of a solid or liquid metal compound with respect to a gaseous environment depends upon its chemical reactivity with that environment or, in the case of an inert atmosphere considered here, its volatility. The physical criterion as to whether or not a particular compound can be levitated is based upon a comparison between those physical properties of the compound determining "levitability" which are defined by the fundamental equations of levitation theory as developed by Okress et a1.,16 and the properties of the metals. Since it is not practical to cover the vast field of metal compounds, further discussion will concentrate on the metal sulfides but the treatment would be applicable to any metal compound. THE THERMAL STABILITY OF METAL SULFIDES The temperatures usually encountered during levitation in inert atmospheres cover the range 1400" to 2000°C. The stabilities of the condensed states of the sulfides under these conditions are considered in relation to the periodic classification by reference to Table I. Two general classes of sulfides emerge. The solid sulfides of elements of group IIB and of groups further to the right are volatile while those sulfides of group IB and of groups further to the left are nonvolatile solids. The sulfides described as volatile may be dismissed as unsuitable for levitation. The stabilities of the more favorable nonvolatile sulfides under the anticipated conditions must be studied more closely From Table I it is seen that the alkali metal sulfides exist as liquids in the temperature range of in-

Jan 1, 1970

By J. H. East

The occurrence of hydrogen sulfide in the gas in solution in the oil produced from the Tensleep sandstone in the Elk Basin oil field in Wyoming constitutes a serious hazard to persons working in, that field. Aware of the general conditions because of petroleum reservoir studies being conducted in that field by its engineers, the Bureau of Mine's willingly agreed to a request of the Petroleum Administration for War to publicize the hazard and the measures for overcoming it. In October 1943 and November 1944, the Bureau of Mines investigated the method's used in handling the oil and in disposing of the hydro¬gen sulfide that occurs with it. This circular reports the results of these observations. HYDROGEN SULFIDE OCCURRENCE IN THE. ELK BASIN OIL FIELD The Elk Basin oil field is in Park County, Wyo., and Carbon County, Mont. It is about 18 miles north of Powell and 12 miles west of Frannie, Wyo. The original Elk Basin oil and gas field was situated in an eroded depression surrounded by an inner rimrock about 200 feet high with a bordering higher plateau about 500 feet above the basin floor.

Jan 1, 1945

By Hoberg H, Schneider FU

The stability of suspensions can frequently be controlled only by the use of supplementary polymeric agents. Such methods date back to the time of the ancient Egyptians, who used natural rubber as a deflocculant for carbon black in the manufacture of ink (Anon, EncyclopediaBritannica, 1968). Since the development of synthetic polymers in the 1950s they have been deployed in all manner of applications. Indeed the mining and paper industries as well as industrial or communal waste water treatment plants are largely dependent on flocculants which make a major contribution to the relief of the environment. As some of the polymers used are carried out from the process via purified water, problems can emanate from the application itself as long as no reliable data is available as to the exact whereabouts of the polymers and their impact on the biosphere. In order not to invade other systems, they would have to be biologically degradable which has not, until now, been confirmed (Blockhaus, Sequaris and Schwuger, 1991; Schumann, 1991). It has, however, previously been demonstrated (Hoberg et al, 1990) that when process water circulates in mineral processing operations, residual amounts of polymeric flocculants can have extremely adverse effects on the selectivity of flotation processes. The adsorption behaviour is consequently one of the most important considerations in the development of new polymers, the aim being to minimise the amount of non-absorbent matter. The objective of the investigations carried out on ampholitic synthetic polymers of high molecular weight to be reported on here was to permit the connection between settling index and adsorptivity to be characterised in greater detail. As the level of knowledge concerning flocculation and polymer adsorption in real systems is still limited in spite of numerous practical and theoretical studies in this field, the experiment was designed to be relatively broadly-based. As well as investigating various raw materials, an attempt was made to compile results on the influence exerted by different surface charges.

Jan 1, 1993

By H. G. Doll

The S.P. log is shown to be a measurement of the potential drop along the drill hole, caused by ohmic effect in the mud. The notion of static S.P. is brought forward, and its relation to the S.P. log is discussed. Other factors influencing the shape and amplitude of the log are considered; attention is given to conditions encountered in practice. Numerous figures are given illustrating graphically the results; these figures are of particular interest for comparison with field examples. The S.P. log, although indicating permeability, is not an absolute measurement of permeability, nor of porosity, of the formations traversed by a drill hole. It is affected by several parameters, such as resistivity of formations and mud, thickness of formations, and others, which should be appraised carefully. Simple rules have been established for a better distinction of the boundaries of permeabl: sections, particularly in difficult cases, such as those encountered in highly resistive formations. A systematic application of the established principles will assist in obtaining more information from the S.P. log than was possible thus far; for instance, under favorable conditions, presence of oil may be detected, or amount of shale in sands may be estimated. Introduction The S.P. log, or spontaneous potential log, has been known and widely used during the last 15 years for the location of permeable beds traversed by drill holes.1,2 In electrical logging practice, the S.P. log is shown on the left hand side track of the record (as may be seen in later examples) where it can be easily correlated and interpreted with the resistivity curves located to the right. Usually, the S.P. log consists of a base line, more or less straight, having excursions or "peaks" to the left. The base line frequently has been found to correspond to impervious beds, while the peaks are usually found opposite permeable strata. Measurements which will indicate positively the presence of permeability in the formations, and which will give accurately the boundaries of the permeable zones, are of great importance in oil-field practice. Thus far, the S.P. log is the best approach to such determinations; unfortunately, its interpretation is not always evident. With respect to the base line of the S.P. log, it may be noticed that this line is not always at a definite location on the chart. Sometimes it may shift abruptly, while other times a gradual drift is apparent. As far as the peaks are concerned, their shape is not uniform; some are rounded while others are sharp. Also, from other data, it may be found that occasionally the peaks extend appreciably beyond the boundaries of permeable zones into zones which are not everywhere permeable. A comparison with permeability measurements made on cores has often confirmed that there was no definite correspondence between the magnitudes of the peaks and the permeability values. In the same geological horizon, it generally will be found that most of the thick and permeable for-

Jan 1, 1949