Search Documents

By George R. Gardner, Kenneth B. Ray

The application of wet cleaning processes for the beneficiation of bituminous coal has created in some localities a problem in the recovery and disposal of fine solids in the washery water. The maximum allowable concentration of these solids in the washery circuit that is consistent with satisfactory operation of the cleaning units remains a controversial point. It has, however, been generally recognized for a number of years that some degree of control should be exerted over the concentration of such material. Early methods of control involved intermittent or continuous discharge of a portion of the plant slurry into near-by streams or settling ponds, and this persisted even after the adoption of settling tanks or cones. The practice is not always economical, for two reasons: first, because of the waste of coal, and, second, because it is sometimes difficult and expensive to obtain an adequate supply of water. The latter condition often is aggravated by chemical treatment of the make-up water that is necessary to prevent excessive corrosion of plant equipment. The modern approach to this problem has been the adoption of continuous thickening devices. However, because such equipment occupies considerable plant space and is somewhat expensive to construct, the practice of loading these thickeners beyond their rated capacity is widespread, therefore often the performance of such units is not altogether satisfactory. In recent years, European washeries have increased the rate of settling of the fine coal from the slurry by the addition of specially prepared starch solutions. These reagents cause flocculation of the solid particles and thereby increase the rate of sedimentation. The first important work on the flocculation and clarification of coal slurry was done by Henry, who developed the Henry process and used it successfully in Belgian preparation plants. Soon after the initiation in Belgium, the process was introduced into England, where subsequent investigation developed similar processes, which were successfully used in

Jan 1, 1940

By G. H. Clevenger

THE reagents now used in flotation consist of various acids or salts, which may be either electrolytes or non-electrolytes, dissolved in water and some substance or combination of substances which function as collecting or frothing agents. At times the only dissolved salts present are those naturally occurring in the water used. The general effect of the electrolyte is to greatly sharpen the separation between the gangue and the concentrate. Examples of this are: The use of sulphuric acid with zinc ores; and of sodium carbonate or calcium oxide (line) with silver-gold ores. Crude pyroligneous acid is also sometimes used when available. Various oxidizing agents, such as permanganates, bichromates, etc., are added in the selective flotation of lead-zinc ores. Many other reagents for performing certain specific functions, either real or imaginary, have been proposed, and a number of them have been tried upon a working scale. The wild orgy of experimentation which is now going on in flotation exceeds even that which followed the introduction of the Washoe process for the treatment of Comstock ores, when, among other things, sage-brush tea and tobacco juice were reagents added to the pans. Out of all this will, of course, eventually come a more or less standard practice for the treatment of each class of ore. Omitting a discussion of the functions of frothing and collecting agents, the reagents used in flotation for this purpose may be classified under five general heads: (1) Essential oils; (2) fixed or fatty oils;. (3) alcohols and their combinations with organic acids; (4) coal tar and its refined products; (5) petroleum and its refined products. A flotative agent of some kind is required in flotation as now practiced. A single reagent, as, for example, certain. of the essential oils, may perform the dual function of frothing and collecting agent, or a mixture of substances may be required.

Jan 9, 1916

By James D. McClung, H. J. Gluskoter, M. R. Geer

INTRODUCTION The purpose of coal preparation is to improve the quality of coal to make it suitable for a specific purpose by (1 ) cleaning to remove inorganic impurities; (2) sizing-crushing or screening, or both; or (3) special treatment, such as dedusting. The properties and quantities of impurities in coal are of major importance in the design and operation of steam generating equipment. Al- though boilers are often designed and equipped to use a wide range of coals, no boiler will perform equally well with all types of coals. All coals have certain properties that place limitations on their most advantageous use. These limitations are especially stringent for many of the older installations. Because of a general lowering of quality of raw coal in recent years, the need for coal cleaning has significantly increased. Among the factors contributing to the need for increased coal preparation are (1) increased demand for quality brought on by market and environmental requirements; (2) increased extraneous dilution caused by mine, health, and safety laws; and (3) depletion of the higher-quality coal seams.

Jan 1, 1979

By Edward Walsh

In the early history of the production of metallic iron from the native oxides or ores, success attended the labors of the workman according to the care he devoted to his work, and according to the degree of skill he possessed in furnishing the required amounts of fuel and ores to be acted upon by the blast propelled by the bellows, trompe, or wooden tub, and delivered into the hearths of the Persian, bloomery, or Catalan forges. The same skill may also have been of avail in the use of the lower forms of the ".Stück," "Blue,"or" Wolf"

Jan 1, 1887

By N. S. Stoloff, M. Gensamer

The effects of temperature, grain size, and magnesium content on the strength and ductility of cadmium were studied in the range -269° to 23 °C. A sharp drop in ductility between -140° and -190°C marked a transition in fracture mode from ductile shear to inter gvanular fracture. The addition of up to 15.35 wt pct Mg in solid solution raised the transition temperature, and for two compositions produced basal cleavages. The relatively high ductility of unalloyed cadmium at cryogenic temperatures is attributed to temperature independence of the yield stress and the absence of dislocation locking. ALTHOUGH numerous studies have been made of the mechanical properties of cadmium single crystals,1-5 no comprehensive investigation of deformation and fracture in polycrystalline cadmium has been carried out. This investigation was initiated to determine the mechanisms of deformation and fracture in polycrystalline cadmium, and to attempt to correlate these mechanisms with the behavior of other metals of hexagonal close-packed structure. A second objective of this work was to determine whether the slip systems and mode of fracture of polycrystalline cadmium could be altered by reduction of the axial ratio, which is 1.886, through alloying. Dorn and co-workers' have been able to induce prismatic slip in magnesium through alloying to reduce the axial ratio. Single crystals of cadmium are so highly ductile that glide strains of 400 pct are observed at room temperature, and 80 pct at -269°c.l Failure in every reported case is by necking down and shearing off of the crystal. Cleavage in cadmium single crystals has never been observed. Magnusson and aldwin reported a ductile to brittle transition for polycrystalline cadmium at about —160 C for specimens tested at a strain rate of 0.05 in. per in. per min in tension. However, even at -196° substantial ductility was retained. The transition temperature was strain rate dependent, impact loading at 19,000 in. per in. per min raising the transition temperature to about -85°C while leaving the low temperature ductility unchanged. No information was given on microstructures or fracture mode, nor were stress-strain characteristics reported. In the present investigation, tensile tests were carried out on polycrystalline cadmium and solid solution Cd-Mg alloys to determine flow stresses, work-hardening behavior, fracture strength, and fracture ductility. Variables employed included temperature, alloy content (and c/a ratio), and grain size.Some compression data also have been obtained for comparison purposes. I) EXPERIMENTAL PROCEDURES A) Polycrystalline Cadmium. Two purities of cadmium were employed in this investigation. Cadmium of 99.95 pct purity was supplied by Belmont Smelting and Refining Co. Cadmium of 99.99+ pct purity was supplied by American Smelting and Refining Co. Threaded cylindrical tensile specimens were machined to give approximately a 1/2 in. long straight gage section with a reduced diameter of about 0.110 in. Specimens were heat treated in evacuated pyrex capsules in the range 140" to 290°C to produce desired grain sizes. All specimens were polished in a solution containing 320 g Cr03 and 20 g NaS04 in 1000 cc of H20. Occasionally this solution caused staining of the specimen, in which case a further polish with a solution of one part HN03 and two parts H202 in two parts ethyl alcohol was employed.' Tensile testing was carried out on a screw-driven Instron machine, at a constant rate of crosshead movement, which for most tests was 0.01 in. per in. per min. Load vs time, and therefore load vs total strain, were recorded. Temperatures from -196" to -40°C were obtained by passing nitrogen gas through a copper coil immersed in liquid nitrogen, and then feeding the gas into a jacket around the specimen. Tests at -269°C were carried out in a helium cryostat, at a crosshead rate of 0.1 in. per in. per min, with specimens of 1 in. gage length. Compression specimens were tested in a jig similar to one designed by ilman. The jig was mounted on the under side of the Instron crosshead. Load was transmitted by means of a rod connected to a movable part of the jig at one end, and the load cell at the other end. A downward movement of the crosshead applied a compressive load to the specimen.

Jan 1, 1963

By H. H. Uhlig

SINCE its first mention in the literature in the eighteenth century1,2 the phenomenon of passivity in metals has stimulated much speculation and attendant controversy as to its nature and cause. No one of the numerous theories so far proposed has been generally accepted. ? Faraday,7 in 1836, associated the passivity of iron with a protective film over the surface of the metal, which materially prevents or slows down reaction with corrosive environments. His theory was that oxidizing acids like nitric acid form an unstable oxygen or oxide layer over the iron surface, which protects the underlying metal from further attack. This concept was simple yet plausible, and without alteration has frequently been assigned in present-day discussions as explanation of the passivity of many metals. With the advent in recent times of stainless steels, it is not surprising that this oxide film theory of passivity proposed by Faraday has been used to explain the phenomenal corrosion resistance of stainless steels and other passive alloys. The passive alloys, such as the chrome-iron alloys, are supposedly covered with a protective oxide film, which forms on exposure of the alloy to air, is extremely stable and self-healing, and accounts for the remarkable resistance of these alloys to corrosion. Within the past few years, several investigators, following the theory of film protection, have attempted to gauge the resistance of the supposed film on steels. Brennert8 and Donker and Dengg9 determined the poten-tial at which a negative ion (e.g., Cl-) moving in an electric field reacted with the metal anode, as detected by increased current flow or change in potential of the steel electrode in an electrolytic cell. The potential corresponding to reaction Brennert called the film break-through potential.

Jan 1, 1939

By A. L. Holmes

Significant technologic advances were made in open pit mining during 1973. The industry faced mounting problems on one front where expansion of stripping activities encountered enlarged public resistance and on another where manpower and materials were in short supply. These challenges, along with the challenge and opportunity to meet the increased demand for mining products including materials for energy production, placed a premium on technical developments and their application. The demands on technology also included the providing of facilities and methods to economically extract minerals from deposits of lower grade, lesser accessibility, and where other uses of land approached the value of its minerals. Detection of Failures in Slope Walls The Bureau of Mines has undertaken research directed towards providing a mine operator with the opportunity to take corrective action before a potential slide becomes a problem.

Jan 2, 1974

By William Phillips

THE earliest mention of the sulphur deposits in what is now Culberson County, Texas, seems to be contained in "Explorations and Surveys for a Railroad Route from the Mississippi River to the Pacific Ocean, United States War Department, 1853-54." Captain John Pope (he was not commissioned Captain until 1856) had charge of one of the divisions of the Survey. In his report on the geology of the route, William P. Blake noted the analysis of a greenish earthy powder from the bed of Delaware Creek, at the springs, which contained 18.28 per cent. of free sulphur. The report states: "From the chemical examination of the waters of the spring, by Dr. Booth, it appears that chloride of sodium is the principal solid ingredient, but considerable quantities of sulphide of sodium are present. * * * * * The waters from the springs examined by Dr. Booth were alkaline, but it is possible that some of the springs are acid; and in this case the precipitation of sulphur would ensue on the mixture of the acid waters with those charged with alkaline sulphurets and the origin of the deposits of sulphur would he thus explained." This is the first reference to the existence of sulphur in that region, the first mention of the character of the water found there and the first suggestion as to the' origin of the deposits. The possibility of the existence of acid waters was confirmed by E. M. Skeats, nearly 50 years later.1 In this publication, Skeats says that the water from the sulphur deposits in Section 11, Block 114,, Township 5, contains 79.08 grains of free sulphuric acid per gallon. This locality is about 13 miles (21 km.) south of Delaware Creek and about 35-miles (56 km.) east of the Delaware Springs. The next published reference to the existence of sulphur in Trans-Pecos Texas is in the First. Annual Report of the Geological Survey of Texas, 1889, page 226, where W. H. von Streeruwitz mentions that sulphur is found in that region, but gives no further information. In the

Jan 9, 1917

By G. M. Ritcey, A. W. Ashbrook, E. G. Joe

Solvent-in-pulp extraction of uranium from acid leach slurries of flotation concentrates is described. Solvent extraction was carried out in a 10 in. diam pulsed-plate column. The extractant was a 0.1 M tertiary amine (General Mills Alamine 336) in a kerosene diluent containing isodecanol as an emulsion suppressor and third phase inhibitor. In pilot plant operation at the Beaverlodge mill of Eldorado Mining and Refining, Ltd., slurry feeds containing up to 35% solids were processed at a throughput rate of 13.5 tpd of dry feed. Uranium extraction obtained was as high as 98%. Amine losses to the raffinate were approximately 0.07 lb amine per ton of original dry feed. The Beaverlodge Mill of Eldorado Mining and Refining employs a carbonate leach for the extraction of uranium from the ore.',' Prior to carbonate leaching sulphides are removed by flotation to reduce reagent consumption. This flotation concentrate containing some uranium is then leached with sulfuric acid, filtered, and the uranium precipitated with magnesium hydroxide. The precipitate is then returned to the carbonate leach circuit. Although the tonnage of flotation concentrate treated by acid leaching is low, reagent costs are relatively high. Also maintenance costs on the acid leach filtration circuit were beginning to show significant increases. The choice of solvent extraction-in-pulp as an alternative to the present circuit was influenced by the following factors: 1) elimination of acid pulp filtration, 2) increase in overall recovery because of soluble loss elimination, 3) reduction of reagent cost (mill sodium carbonate solutions are used as strip), and 4) production of higher purity precipitate at the mill site. Because a solvent-in-pulp process would be difficult to test on a bench-scale, the Eldorado experience in the use of pulse columns,3-5 mixer-settlers,6 and solvent-in-pulp operations in particular7 was applied directly to the initial pilot plant carried out during the summer of 1965 and followed by the second pilot plant in 1966. The latter work, which is presented in this paper, determined the following factors for anticipated scale-up to plant production: 1) overall uranium recovery by this process, 2) tonnage throughput expected, and 3) solvent losses anticipated for the full-scale plant. The equipment used consisted of a 10 in. diam extraction pulse column and three mixer-settlers for scrubbing, stripping, and acid equilibration. All equipment was designed by Eldorado and much of the pilot plant was built at the mill site. PROCESS CHEMISTRY Feed to the acid leach plant consists of a sulphide flotation1,2 concentrate containing mainly pyrite, uranium and graphite, with a particle size of 90%

Jan 1, 1968

By J. Handin

Triaxial compression tests with independently applied external confining pressures and internal pore pressures show that the ultimate compressive strengths of representative oil well cements are nearly linear functions of effective pressure — the difference between external and internal pressures on the jacketed cylindrical specimens (to 15,000 psi). The strengths are little affected by the test temperature to 350F (not to be confused with the curing temperature). At an effective pressure of 15,000 psi, strengths are in the rage of 30,000 to 50,000 psi, comparable to those of sedimentary rocks under similar conditions. The cements become very ductile even under low effective pressures; permanent shortenings of 30 per cent or more are attainable without rupture. INTRODUCTION Since the pioneering work of Richart, Brandtzaeg and Brown1 on the failure of cement under combined compressive stresses, it has been recognized that ultimate compressive strength is greatly enhanced by the application of confining pressure. More recently, Mc Henry2 showed that the strength of concrete was a linear function of the effective pressure (the difference between the external confining pressure on a jacketed specimen and the internal fluid pore pressure), at least for a range of 0 to 1,500 psi. The effect of temperature had not been investigated, and no previous systematic triaxial compression testing of naterials used for oilwell cementing seems to have been done. The present work was suggested by the late J. hi. Bugbee3 who stated that "consideration of the common application of high-pressure hydraulic fracturing to the initial completion or recompletion of wells, and the large pressure drawdowns in some producing wells, particularly those in abnormally high-pressure gas-condensate reservoirs, raises the question of what is a suitable cement strength for various completions. The intuitive belief exists that cement strength need be no greater than formation strength. Tests should, however, be conducted at downhole conditions." The ultimate compressive strengths of rocks penetrated by the borehole must rise several fold with increasing depth.4 This marked enhancement of strength is due to the influence of the effective pressure, the total weight per unit area of the overburden less the hydrostatic pore pressure. (The effect of temperature due to the geothermal gradients is relatively small for depths to 30,000 ft.) .A significant comparison of the strengths of rocks and cements at downhole conditions requires knowledge of the confined compressive strengths of cements as well. EXPERIMENTAL PROCEDURES The theory and technique of triaxial compression testing are fully discussed in earlier reports.4-6 Briefly, cylindrical specimens 1-in. long and 0.5-in. in diameter are jacketed in thin copper tubes of negligible strength, placed in the test chamber and subjected to an external confining pressure of kerosene and loaded axially by the piston at a strain rate of 1 per cent per minute. Pore pressures of water (or kerosene) are applied independently through the hollow piston and are maintained constant during the shortening of the specimen, Tests at sensibly 0 pore pressure are arranged so that any free water in the cement can escape to the atmosphere. (If egress of water were denied, pore pressure would rapidly attain the value of the external confining pressure because of reduction of pore space.) The test chamber can be heated for high-temperature experiments. Unless otherwise noted, the cement samples were air dried for about a week. Recorded during a test are pore and confining pressures, shortening and axial differential force (total force less the product of the confining pressure and the area of the piston). True stress-strain curves are constructed by dividing the measured differential force by the actual cross-sectional area of the specimen at a given

Jan 1, 1966

INCREASING realization that pouring and ingot-mold practices involve many factors of fundamental importance to ingot quality and general steel-mill operations has caused these phases of steelmaking to become major concerns of operators and metallurgists engaged in control of quality and costs. Methods of pouring steel from the ladle into the ingot molds have some direct effects on ingot quality. The mold itself governs solidification and dimensions of the ingot and in so doing exerts some very tangible influences not only on ingot quality but also on product yields and general steel-mill processing. In addition, practices are employed in the handling of molds during daily open-hearth operations that are important to quality and production costs. Therefore, pouring and mold practices must be considered highly specialized and important steps in steel-mill operations. MOLD DESIGN Mold design is difficult to discuss in a precise manner because it varies greatly throughout the industry, both in theoretical concepts and practical application, and few well developed data are available. Most ingot molds are designed to meet conditions peculiar to a given plant wherein quality standards are dictated by end-use requirements, which may differ considerably even for the same grade of steel. The mold designer must also consider the equipment available to process ingots and the product obtained from them. Such equipment, used for stripping, heating, blooming and finishing operations, is seldom, if ever, exactly the same in any two steel plants. Thus, pronounced contrasts in mold designs can be expected to continue, even among plants making strictly comparable types of product, particularly because some producers are just beginning to realize the benefits possible from specialized designs. Certain fundamentals are used in mold design but even these

Jan 1, 1964

For the convenience of members who may be trawling from place to place, the Secretary has compiled a list of libraries or other places in the United States and foreign countries here MINING AND METALLURGY or the Transactions may he consulted. This list will be sent to members if they so request.

Jan 1, 1923

For the convenience of members who may be traveling from place to place, the Secretary has compiled a list of libraries or other places In the United States and foreign countries where MINING AND METALLURGY or the Transactions may be consulted. This list will be sent to members if they so request

Jan 1, 1923

The total number of applications brought before the Committee during the year 1916 was 962; the total number, of persons who were elected, and became members of the Institute during the wane period was 750. The total membership of the Institute on. Dec. 31, 1916, was. 5,781, consisting of 19 Honorary Members, 5,246 Members, 215 Associate Members, and 301 Junior Members. The changes in membership during the year are shown on the accompanying schedule:

Jan 2, 1917

By Bernard MacDonald

Of the treatment of the slime-pulp of gold- and silver-ores by cyanidation, agitation is an essential part. When prepared for treatment, this pulp, consisting of ore reduced to such fineness that approximately 80 per cent. of it will pass through a 200-mesh screen, is mixed with a certain proportion of water, carrying in solution the cluantity of cyanide (KCN) and other chemicals required. The water-constituent of the pulp thus prepared usually ranges from 1 to 2 parts by weight to 1 of the dry ore. Thus constituted, the pulp is charged into treatment-tanks, the shape and capacity of which vary, according to the quantity of pulp to be treated daily and the method of agitation to be employed. Tanks have no other function in a cyanide,plant than that of being economical and corlvellient containers or receptacles for holding the pulp, solutiou, or water used in the operations. It is by agitation that the solids in the pulp charged into the tanks are kept in suspension in, and mixed with, the solution in the proper proportions required for the treatment. If the proper mixture of solution to dolids be determined to be 2 to 1 by weight (which is, approximately, 5 to 1 by volume), this proportion should be maintained in every part of the charge; that is, each solid particle of the pulp, whether it be of' 180- or 400-mesh size, should be surrounded by five times its own volume of solution throughout the whole period of treatment. The reason is, that the amount of chemicals ascertaiued to be necessary for dissolving the gold and silver contained in the solids, is held in uniform solution in the water-constituent of the pulp, and, therefore, the determined proportions of solution and solids must be maintained at all times during treat-

Jan 1, 1912

By Richard E. Lounsbury

Coal mine refuse handling traditionally has been the redheaded stepchild of the industry-a problem to be ignored as much as possible. During the past few years, however, mining companies have become more aware of the potential water pollution problem associated with refuse handling and storage. Planning for refuse disposal involves environmental protection and the economics of refuse handling. For over two years, Monterey Coal Co. has operated a non-polluting refuse disposal system at its No. 1 Mine located in Brushy Mound Township of Macoupin County 6 miles south of Carlinville, Illinois. Drainage goes to Spanish Needle Creek and eventually to the Illinois River. The mine produced 3.5 million tons of clean coal during its first two and one-half years of operation and is designed to produce 3 million tpy of clean coal at capacity.

Jan 6, 1973

By J. T. Eash, N. B. Pilling

As a group, the alloys of iron, nickel and carbon are, in application, one of the most versatile of the ferrous alloy family, and while many investigations have been made of their properties and structure only a few attempts have been made to show the microstructural relation over a wide range of composition. It is necessary at once to be clear about the kind of structural relation with which we are concerned. The equilibrium diagram provides quantitative data regarding structural make-up and its variation with temperature, but equilibrium structures often are far different from the technologically significant ones. This is particularly true of steels and cast irons, and some of the most important components of their structure may have no place in the diagram of equilibrium. The fugitive phases that result from transformation are dealt with in a highly detailed and descriptive manner in the S-curves originated by Bain. The present effort lies in a still different field, which is to portray the relation between sweeping changes in composition and in resultant structure, under controlled but nonequilibrium conditions of thermal treatment. The Guillet1 diagram presented in 1903 was the initial attempt at such a correlation and frequent references to this diagram can be found in the literature even though later work has shown it to require considerable modification. Kase2 published in 1925 a diagram that was based upon observations of furnace-cooled melts. At low carbon contents this diagram agreed fairly well with experience in showing pearlite to exist in alloys containing up to 6 per cent nickel, and completely austenitic steels at 24 to 28 per cent nickel. At high carbon contents, however, irons were indicated as being martensitic at around 2 per cent nickel and austenitic at 12 per cent nickel; these interpretations are open to serious question. Based upon experience with steels and cast iron, Wickenden3 suggested a diagram that agreed fairly well with Kase's in the steel range but which presented a wide departure from it in the higher-carbon, high-nickel regions. In its broad picture, the Wickenden diagram is an approach to "practical" structures. [ ] Reference may be made at this point to the efforts of Marshy to construct an iron-nickel-carbon equilibrium diagram by the coordination of scattered data, which are described at length in the monograph cited. None of these preceding attempts has appeared to meet the need for an exposition of the structural sequence that is encoun-

Jan 1, 1942

By J. W. Hickman, E. A. Gulbransen

One of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film. A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film. A comprehensive program has been undertaken to study these phenomena. This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C. Before the introduction of the electron diffraction technique, it was necessary to use either direct chemical analyses or X-rav diffraction analyses to determine the nature of the oxide film formed on the metal or alloy. Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry. In special cases the information obtained may be identical, but in general both viewpoints are necessary. Much of the early work was carried out on the oxidation of bulk samples where thick films were obtained. The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses. Although much useful information has been obtained in this manner. little could be learned about the character of the protective oxides during the period when the films were actually protective. Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique. In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective. Literature The oxidation of iron has been extensively investigated by X-ray and electron diffraction. Jackson and Quarrelll found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature. The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe³O4; between 515° and 900°C. the stable film was FeO. Above the upper change point of iron the oxide was found to be Fe³O4. From 400' to 515°C., FeO, Fe³O4 or a mixture of the two oxides was found. Recrystallization of the air-formed film below 400' and above 900°C. led to the formation of Fe3O4. In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described.

Jan 1, 1947

By E. A. Gulbransen, J. W. Hickman

One of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film. A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film. A comprehensive program has been undertaken to study these phenomena. This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C. Before the introduction of the electron diffraction technique, it was necessary to use either direct chemical analyses or X-rav diffraction analyses to determine the nature of the oxide film formed on the metal or alloy. Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry. In special cases the information obtained may be identical, but in general both viewpoints are necessary. Much of the early work was carried out on the oxidation of bulk samples where thick films were obtained. The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses. Although much useful information has been obtained in this manner. little could be learned about the character of the protective oxides during the period when the films were actually protective. Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique. In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective. Literature The oxidation of iron has been extensively investigated by X-ray and electron diffraction. Jackson and Quarrelll found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature. The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe³O4; between 515° and 900°C. the stable film was FeO. Above the upper change point of iron the oxide was found to be Fe³O4. From 400' to 515°C., FeO, Fe³O4 or a mixture of the two oxides was found. Recrystallization of the air-formed film below 400' and above 900°C. led to the formation of Fe3O4. In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described.

Jan 1, 1947

By G. O. Hiers

THE object of the experiments reported in this paper is to determine the eutectic composition of copper and tin and to determine the location of the part of the liquidus line immediately above the eutectic composition in copper. Three methods were used in the investigation: (1) the method of dissolving copper in a bath of molten tin at constant temperature, with the idea that when the bath was saturated with copper its copper content, by analysis, together with the temperature at which the saturation took place would locate a point on the liquidus line (2) the method of the differential cooling curves, and (3) the method of microscopic examination. This paper is principally concerned with the results of the last two methods mentioned. The results of the first method, that of dissolving copper in molten tin, did not agree with the .results of Miller,1 by the same method, nor with the results of other investigators by other methods, nor yet with the results of the cooling-¬curve experiments and microscopic examination reported here.

Jan 1, 1929