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By B. M. Larsen, W. E. Shenk

This paper describes a method of reversal control of the open-hearth furnace that obtains in practice those effects considered below as essential to a completely automatic control, without appreciable interference with the natural rise and fall in temperature of the regenerative portions of the furnace system. Growing out of some studies of radiation pyrometry in open-hearth regenerators, it was developed during 1934-1938, and has been successfully applied to a number of commercial furnaces. The goal of open-hearth furnace operation is the highest rate of production of steel of proper quality consistent with good refractory life and fuel economy. This requires rapid heat transfer from furnace to charge, which in turn is dependent upon heating the furnace refractories to the highest safe operating temperature. The greater the heat input to the melting chamber, the sooner this limiting temperature will be reached, so that control methods in general that are designed to protect against overheating of refractories should help to maintain maximum fuel input and production rate. For the typical open-hearth system, with fixed regenerator capacity and with rate of fuel input usually restricted in its range of variation, our basic assumption is the idea that the only other important variable —that is, the time interval between successive reversals—should also be held constant or within a small range. The present reversal control was designed therefore so that, under normal operating conditions, no arbitrary limitation is imposed other than to keep the reversal interval within the optimum time range. However, since a near approach to completely automatic operation involves protection of refractories through the balancing of furnace end temperatures as well as emergency protection against temperature peaks above some upper limit, it was also felt essential to employ, as an integral part of the control unit, a temperature-measuring instrument to register the true temperature of the refractory surfaces at some critical region in the hot ends of the regenerative zones. As the basic elements of the control, we thus have one "maximum" and one lLminimum" time relay and a potentiometer recorder-controller, combined with switches and relays to operate as follows: I. Reversal normally occurs within an optimum range limited by the maximum and minimum settings to about 4 to 6 min. variation, but the actual interval usually is less variable and closer to the minimum setting. 2. The margin between minimum and maximum time is utilized, together with a "floating temperature limit" in the potenti-ometric control instrument, to correct any tendency toward temperature unbalance between ends of the furnace. 3. A second "maximum temperature

Jan 1, 1945

By David R. Mitchell, E. A. Reilly, G. R. Gardner, F. P. Lasseter

THE methods that may be applied to the treatment of slurries and water, as these are related to practical coal-preparation problems, are concerned essentially with the movements of solids suspended in water. It is assumed that there are no fundamental differences between the principles involved in the treatment of coal slurries and the phenomena encountered in general mineral-dressing practice, and the latter are-presented in some detail. Basic principles are correlated with present practice for both the anthracite and the bituminous coal fields, and methods are discussed which are designed to utilize best all the material subjected to treatment and suggest a sound approach to the solution of problems relating to the return of clear water to process or to streams. In order to approach the practical phases of the subject with sufficient understanding of the basic principles, it is necessary to discuss two types of phenomena that are applicable. The first is flocculation and the second is sedimentation. Descriptive matter is given covering the various methods and types of equipment employed to conduct these operations, with emphasis on their application to water and coal-slurry treatment. DEFINITION OF TERMS Definitions of terms are consistent with modern developments, and conform, in general, with their usage in mineral-dressing practice. Because of variations in coal-preparation methods, it is impossible to define a rigid upper limit of particle size for a coal slurry or sludge which will apply generally. Limits vary somewhat with the particular treatment method employed at a given plant. For purposes of definition, this limit is chosen as the particle size for which preparation methods such as Chance comes and jigs are usually dispensed with, and other methods, such as the Hydro-tator, tables, and froth flotation, are employed. Generally the limit will be 10 to 6 mesh.

Jan 1, 1950

By A. H. Daane, R. L. Myklebust

The yttrium-manganese system has been investigated by thermal, metallographic, and X-ray diffraction methods. There are three intermetallic compounds present: YMn2 which melts congruently, YMn4, which undergoes syntectic decomposition, and YMn,, which undergoes peritectic decomposition. The compound YMn4 is ferromagnetic at room temperature with a Curie temperature of 214°C. There are eutectics at 25.2, 60.9, and 82.0 wt pct Mn which melt at 878°, 1100°, and 1075°C, respectively. Crys-tallographic data are given for YMn4, and YMn12 . The terminal solid solubilities are low. In a general program of study of yttrium metal in this laboratory some alloy systems of this metal with elements of the first transition period have been examined. This work was originally instigated by experiences in cladding yttrium with jackets of some protective metals such as Inconel for high-temperature service in air.' In some cases a low-melting phase was observed to form between the Inconel and the yttrium resulting in failure of the samples. In characterizing this reaction, a survey was made of the systems of yttrium with chromium, manganese, iron and nickel,, and it was found that a eutectic was formed between these metals and yttrium on the yttrium-rich side of the system. This present study of the Y-Mn system was carried out to examine in more detail the alloying nature of yttrium, and to correlate trends that have been observed in previous related studies. It was observed by Voge13 that in the systems of lanthanum, cerium, and praseodymium with each of the metals in the first transition series, the tendency to form compounds diminished in the order nickel, cobalt, and iron while no compounds were formed with manganese, chromium, or titanium. Beaudry and Daane4 observed a similar behavior in the systems of yttrium with some members of the first transition series except that the tendency for compound formation was greater. Both the Y-Ti5 and Y-Cra systems consist of simple eutectics, while in the Y-Fe,7 Y-CO, and Y-Ni4 systems, there are four, eight, and nine compounds, respectively. In addition to the above trends, the similar atomic radii and electronegativities of yttrium and thorium invite a comparison between their alloying behaviors with a common element such as manganese. In crys- tallographic studies, Florio et al.' have identified three intermediate phases in this system which are ThMn2, Th6Mn23, and ThMn,,. Gschneidner and Waber10 have examined published information on alloy systems of the rare-earth metals and have correlated this information with current alloying theory. From their study, they predicted that the Y-Mn system would contain one intermetallic compound. On the basis of this prediction, the trend in the alloying behavior of yttrium with the elements of the first transition series and the alloying behavior of thorium with manganese, one might expect from one to three intermetallic compounds to form in the Y-Mn system. A consideration of Hume-Rothery's rules of alloying based on size-factor, electronegativity, and valency suggested a small terminal solubility and possible compound formation. The present study was undertaken to confirm these predictions of low terminal solid solubility and compound formation and to establish the general alloying behavior of yttrium with manganese. EXPERIMENTAL Materials. The manganese used in this investigation was obtained from the Foote Mineral Co. as electrolytic plates of 99.9 pct stated purity; the yttrium metal was prepared in this laboratory. Table I gives the analyses of these materials. For the solubility studies at the yttrium-rich end of the alloy system, distilled yttrium, whose major impurity was 200 ppm Ti, was used. Preparation of Alloys. The alloys were formed by comelting the two metals in an are-melting furnace under an atmosphere of argon. The buttons thus formed were inverted and remelted three to five times to promote homogeneity. Due to the high vapor pressure of manganese, it was assumed that the weight lost during are-melting was all manganese. This assumption was based on the very good agreement observed between calculated compositions and chemical analyses of several alloys. The compositions of the dilute alloys used for solid solu-

Jan 1, 1962

By G. P. Gladis, R. H. Atkinson

Palladium has been used for jewelry for many years, particularly in conjunction with gold. This use increased in amount during the war, as palladium and gold were only moderately used for war purposes while demands for platinum and some of the other members of the platinum group were so great that their use in jewelry was prohibited. Palladium hardened with a small percentage of ruthenium has the necessary technical properties and appearance for good jewelry, and it is sufficiently rare to be desirable for luxury items—at least I00 times as rare as gold. Although both visual and spectro-photometric examination demonstrated that the color of Palladium was almost the same as that of platinum, a few jewelers found the surface of palladium, even after some polishing, rather dark in areas that had been repeatedly heated during the soldering necessary to assemble certain types of handmade ornaments. This phenomenon is not to be confused with the thin, bluish oxide film that can be produced by heating in air over the range 400' to 800°C., as that film is easily reduced by dipping in warm 5 per cent formic acid or in warm methanol. It was suspected that the difficulty arose from heating in atmospheres that were alternately oxidizing and reducing, as Wise and Vines1 had found that this opened the grain boundaries of palladium and palladium-silver alloys in the same manner as in pure silver, as reported by Martin and Parker.2 This damage is caused by the reaction between oxygen in solid solution in the metal, acquired when heated under oxidizing conditions, and hydrogen diffusing in from subsequent heating under reducing conditions; the steam cannot diffuse out and therefore builds up sufficient pressure to disrupt the metal near the surface. Copper and various other metals can be damaged similarly, but platinum is nearly immune; therefore the problem was new to the platinum jeweler. Sulphur in the fuel gas also can cause trouble but did not appear to be dominant in the present instance. Metallographic examination of both pure palladium and ruthenium-palladium showed that the usual torch using oxygen and city gas as normally operated did in fact cause the surface and subsurface damage that had been observed, and also disclosed that a reducing flame caused more damage than an oxidizing flame and was very damaging even in the absence of any intentional swing in atmosphere from oxidizing to reducing (Fig. 7); besides the surface damage, there was serious loss of ductility. A full explanation of the mechanism of attack is not evident at the moment, but may be allied to the attack that occurs on heating catalytically active metals in nonequilibrium atmospheres.

Jan 1, 1946

By Robert Linton

Tats paper deals with work that has been carried on for over three years by the management and staff of the North Butte Mining Co. in an effort to standardize mining methods, to eliminate lost motion in the operating organization, and to improve the efficiency of the individual workman. Naturally, much of this work is an adaptation of ideas suggested by other mining operations or by practice in manufacturing and other productive industries. The studies, however, have developed some features that it is believed are new. Both new and adapted features are given in detail. The normal capacity of the North Butte mines is about 2000 tons per. day. Hoisting is done principally through the Granite Mountain shaft, which is 3740 ft. (1140 m.) deep and equipped with an electric hoist capable of hoisting 200 tons per hour from a depth of 4000 ft. (1219 m.). The lowest stoping level is the 3400-ft. The Granite Mountain shaft is connected with the Speculator shaft, about 850 ft. (259 m.) south, and with the Gem, about 1150 ft. (350 m.) east, which are 3000 (914.4 m.) and 2000 ft. (609.6 m.). deep, respectively. These two shafts are equipped with reversible fans for ventilation. The Speculator has a; steam hoist with a capacity of 150 tons per hour from the 3000-ft. level. The Granite Mountain shaft is concrete lined from the 1600-ft. to below the 3000-ft. level and gunited with cement from the 1600-ft. level to the surface. Sections of the Speculator shaft with a total combined length of 500 ft. (152.4 m.) are also concreted. There are approximately 36 miles (58 km.) of drifts and crosscuts in the mine, in which there are 15.2 miles (24.5 km.) of track. At normal capacity, about 75 stoping faces, 20 raises, and 30 sill development faces are working. Stoping is usually by the standard square-set method. Where the size of the oreshoot and character of. the walls permit, the rill (or cut-and-fill) system is employed.

Jan 8, 1920

By J. P. Pritchard, J. T. Pierce, O. G. Slay

This paper discusses the results of a technology-evaluation program to ascertain the feasibility of a piotornask-photoresist technology developed for fabrication of multiple-layer thin-film superconductive circuitry. The uehicle selected for this evaluation was a 120-bil associative data processor requiring a set of nine photomasks to define a similar number of patterned material layers of lead, tin, and polymer insulation. A total circuit area of 4 sq in. involved 2500 actitle and 12,000 passive crossings. Several short-free, electrically continuous specimens were satisfactorily completed under this program. Problems encountered in the preparation and use of the requi-ed set of Photomasks are discussed, as also are the problets of providing suitable external connections. A major retarding factor in the development of the superconducting thin-film cryotron technology for many years was the absence of batch fabrication means yielding necessary device density and count per substrate for practical applications. Early workers in the field desired only limited numbers of devices to permit careful study of discrete devices and representative circuitry integrating logic and memory capabilities. For these purposes mask stencils could be formed to selectively control the placement of materials, sequentially vapor-deposited in vacuum, to form the multilayer structure. In general a distinct pattern was required for each material layer; therefore, mechanical provisions were required to change not only the material source, but the patterning mask as well, before each deposition. All deposition steps were preferably performed in a single evacuation of the deposition chamber. Thus the means for storing, transporting, and registering masks and sources with respect to the substrate existed and were operated within the vacuum environment. In the authors' experience, the approach was and remains serviceable for preliminary device study, but was not extensible to an economical manufacturing method by virtue of the difficulties inherent in mask stencil preparation and use, and the capital investment implicit in the mechanization requirements. Since the commercial attraction of the cryotron technology stems principally from its potential for economical batch fabrication, the authors' program has placed major emphasis on fabrication methods. A highly useful method has evolved through adaptation

Jan 1, 1967

By M. E. Wadsworth, L. H. Raby, A. S. Peck

Infrared spec troscopy was used to study the adsorption of oleate collector on three varieties of hematite. Each of the minerals was found to react with either oleic acid or a solution of sodium oleate to form a mineral cation-collector anion chemisorbed layer at the solid-liquid interface. The chemisorption reaction displaced surface hydroxyls and was found to be pH dependent. The infrared band characteristic of the antisymmetrical C = 0 structural group of chemisorbed oleate appears between 1520 and 1540 cm-'. Evidence is presented which shows that molecular filming of the mineral surfaces with un-dissociated oleic acid precedes chemisorption. Infrared absorbance is correlated with the flotation behavior of the mineral. Adsorption processes are usually classified into two types which are distinguished and character- ized by the nature of the bond formed between the adsorbate and adsorbent. The process in which molecules chemically bond to solid surfaces is termed activated adsorption or chemisorption. If only weak van der Waals forces bind the molecules to the surface then the process is termed physical adsorption. Chemisorption is of primary interest in flotation systems since selectivity may be obtained if a single mineral is rendered air-avid by a specific collector mineral adsorption reaction. In previous studies infrared spectroscopy was used to define the mechanisms involved in the adsorption of oleic acid and sodium oleate on fluorite, barite, and calcite. Infrared techniques were particularly useful since adsorbed monolayers were identified in situ. Further, the infrared method permitted identification of reaction products in the solid, liquid, and vapor phases of the systems. The chemisorption reactions displaced F- from fluorite, SO4 from barite, and CO3 from calcite. This investigation was pursued in an effort to characterize and interpret the adsorption processes for synthetic hematite, compact red hematite, and specular hematite (crystalline hematite). Adsorption tests were performed using either oleic acid or

Jan 1, 1967

By H. E. Brauer

PART I INTRODUCTION Among the zinc base alloys used for casting in metal moulds, particularly die casting, those alloys containing aluminum usually together with copper, are probably the most widely used. The reason lies in their desirable mechanical properties and the fluidity and absence of hot shortness which facilitate casting. Objection to the use of these alloys may bee raised on account of the rather frequent instances of failure of a type variously described as disintegration, exfoliation and intercrystalline corrosion. In all cases which have come to our knowledge where the conditions of service were known, failure has occurred upon exposure to moisture and heat varying from a hot moist atmosphere to high pressure steam. Moreover, the alloys described in all such cases contain impurities or alloying metals which the present authors have found to have enormous accelerating effects on intercrystalline oxidation in zinc-aluminum alloys. Thus Williams1 experimented with an alloy containing a large percentage of tin exposed in Cuba. Bauer2 reports failure of a boiler plug containing over 1 per cent. of impurities, doubtless lead for the most part, and Rawdon's3 examinations were made on an alloy containing 0.4 per cent. lead also exposed to the Tropics. No thorough investigation of the nature and cause of this type of failure has been made heretofore, so far as the authors are aware, although Rawdon correctly classified it as internal oxidation. We have, therefore, carried out this investigation in order to determine the exact nature of this phenomenon and the effect of other metals present as impurities or intentional additions in accelerating or-retarding it. In the appendix we include a considerable amount of data which may be valuable in selecting an alloy combining good physical properties with high resistance to oxidation.

Jan 8, 1922

By Henry Hebley

IN preparing this paper it has been the aim of the writer to keep the problems of both producers and consumers in mind. Until now, no attempt has been made to familiarize each group with the other's practice and limitations. This paper is an effort to acquaint the readers with some of the factors pertaining to the problem and cost of mining and preparing steam coal, and also to the economics of producing steam with such coal. In recent years all lines of endeavor have turned to intensive mechani-zation in order to lower the unit cost of production. The average fuel consumption in steam electric generating stations has dropped in 20 years from 4.0 lb. to 1.4.1b. per kilowatt-hour; while the modern power station can generate 1 kw-hr. on a fraction under 1 lb., or 13,000 B.t.u. coal. Also, the amount produced per man has in that same period risen from 3.8 to 8.2 tons, owing to the use of modernized equipment below ground for coal cutting, drilling, shooting, loading, hauling and hoisting. Unfortunately, the rapid speed of 5 tons per minute of operation at which the coal is loaded mechanically precludes any appreciable removal of impurities at the coal face, so that the raw coal is hoisted containing a markedly higher percentage of impurities than the hand-loaded coal, which was subjected to the scrutiny of the miner during loading. Also, during the past 20 years, certain seams of coal lying close to the surface have been made economically available by the improved design of electrically operated shovels and draglines for the removal of overbur-den running as high as 56 ft. This strip coal frequently contains so much ash in the raw state (Table 1) that it would have no sales value. There-fore, coal preparation must be adopted to beneficiate the raw product. Some seams in the United States have a decreasing ash content with decreasing size, owing, in all probability, to the fact that the coal is friable while the impurities are hard, causing a concentration of the low-ash material in the fine sizes. Illinois No. 6 coal being rather hard, naturally the reverse is true.

Jan 1, 1937

By Ivor Jenkins

PROCESSES employing controlled atmospheres in the heat-treatment of metals and alloys are now well established on an industrial scale, and the general principles involved and the advantages to be gained in the use of the technique have received considerable publicity over a period of years. During this time the greatest emphasis has been on the establishment of the process in industry, the main effort being devoted to development work on various types of atmospheres, their useful fields of application and the design of suitable heat-treatment furnaces in which they are to be used. The various types of controlled atmospheres are fairly well standardized, but there still remains a considerable field for the investigation of related problems, in connection with both the gas-generating equipment and the surface chemistry of the heat-treatment of metals, especially in complex controlled atmospheres. This paper describes certain investigations of this nature that were carried out in England up to 1939. The development of processes employing controlled atmospheres has been associated to a very large extent with the heat-treatment of steels, both because of the major importance of steel in industry and the many diverse and difficult problems of surface chemistry involved when steels of such a wide range of composition are heated in the presence of active gases Controlled atmospheres such as dissociated and burnt ammonia or charcoal gas are used in the heat-treatment of low-carbon and high-carbon steels, but from certain points of view a suitable atmosphere generated by the partial combustion of city gas is to be preferred. Both the ammonia derivatives are comparatively expensive, and even if the burnt ammonia is regenerated, thereby reducing operating costs, the capital expenditure of the gas plant may make it prohibitive for the smaller type of furnace installation. Charcoal-gas generators are not without their operating difficulties: especially those associated with the quality of the charcoal, clinker formation and the removal of carbon dust from the generated gas. City gas has the advantage of being comparatively cheap and "on tap" in most if not all industrial centers. The use of raw city gas as a protective atmosphere in the heat-treatment of steels has been described,1 but it presents certain difficulties because of its complex composition and its explosive nature when mixed with air. These factors, together with the tendency toward sooting at elevated temperatures, arising mainly from the hydrocarbon gases present, all militate against its use as a protective atmosphere in industrial furnaces. The following analysis, based on the analyses of city gas in different localities in Great Britain, indicates the wide limits existing

Jan 1, 1947

By Raymond D. Sloan

Development and exploration in Oklahoma showed a definite increase in 1941 over 1940 in production, wildcat activity and total well completions. Geological and geophysical work continued and possibly increased slightly in amount. Oklahoma retained third place in the ranking of oil-producing states of the nation, topped only by Texas and California, and followed by Illinois in fourth position. Production averaged 416,800 bbl. daily, a 1.7 per cent increase, as compared with 409,900 bbl. daily for the year 1940. Maintenance of the state's relatively stable producing rate resulted from the discovery of numerous small pools, the recombing of old areas, the establishment of new producing horizons, and the drilling of an increased number of marginal wells. The market for the Mid-Continent crude was strengthened materially to meet the increased demand. Coincident with a deeline in production in Illinois, shipment of Oklahoma-Kansas crude to the eastern points averaged 453,000 bbl. per day, an increase of 49.4 per cent as compared with 1940. The movement south amounted to an average of 42,000 bbl. per day, a loss of 41.7 per cent. Secondary-recovery programs in Oklahoma were given more consideration, operators realizing that in the future many pools would necessarily have to resort to this type of operation. Five permits for water-flooding were issued by the Corporation Commission during the year. These projects were in Rogers, Wagoner and Nowata Counties, in the shallow northeastern area, which has relatively extensive development of this type in the Bartles-ville sand at from 600 to 1000 ft. in depth. Gas repressuring of an individual lease in the 35-year old Glenn pool, Creek County, proved relatively successful, and after a year's operation was extended to cover a much larger area, with several operators participating. More of this type of work is expected in the future; however, it was given an initial setback when the legislative proposal authorizing secondary recovery in the Wilcox zone of Oklahoma's largest pool, the Oklahoma City pool, was pigeonholed by the committee. A continuation of the low discovery rates within the state would possibly lead to a revival of interest in the project. Many pools formerly classified as prorated areas were removed from this classification and transferred into the group of settled production. At the close of the year the issuance of the Federal Conservation Order M-68 and the interrelated Preference Rating Order P-98 caused a sharp decline in drilling operations, which is expected to continue until such operations are stabilized at a lower rate. The ultimate effect of these two orders on discoveries, production and reserves is a matter of speculation and conjecture. During the year, 2110 new wells were drilled, an increase of approximately 18 per cent as compared with the previous year. Of the total, 1235 were oil wells with a combined initial potential of 342,754 bbl. daily, 178 were gas wells with a total

Jan 1, 1942

By Bernhard Blumenthal

A melting process was developed by which high purity electrolytic uranium crystals can be converted into sound ingots without serious contamination. Careful preparation of the crystals, melting in a high vacuum, and directional solidification led to a metal of better than 99.993 wt pct purity. The metallographic examination showed a substantially clean metal with only residual amounts of a second phase which responded to heat treatment. The density of high purity uranium is 19.05 g per cu cm. FOR the study of the fundamental properties of uranium and its alloys, a base metal of high purity is needed, and an investigation was started at Argonne several years ago to examine various methods of preparing high purity uranium. Early success was achieved by the fused salt electrolysis process in preparing high purity metal in crystal form,' and the problem became that of melting the crystals into ingots without contamination. The electrolytic crystals contained a few ppm of heavy metals, less than 15 ppm C, and large quantities of potassium and lithium in the form of trapped fused salt electrolyte. On melting in vacuo in magnesia or urania crucibles, the metal picked up considerable quantities of carbon and some iron, copper, and silicon but lost most of the potassium and lithium. It was not metallographically clean, and much research work was necessary to determine the optimum melting conditions for minimum contamination. This work has resulted in the development of a melting procedure by which sound ingots can be prepared with only a limited contamination by carbon. In the section entitled "Melting of the Electrolytic Metal," the equipment and processes that have been developed for melting the electrolytic crystals are described in detail. The "Metallography" section is devoted to the metallography of high purity uranium, and the section "Density of High Purity Uranium" contains the first property measurement on high purity uranium—a density determination. Melting of the Electrolytic Metal Apparatus—Melting and Vacuum Equipment: Uranium may be melted in either resistance or induction-type electric furnaces. Resistance heating was found to be preferable to induction heating for melting down the electrolytic crystals, for several reasons: Although induction heating permits fast heating, this advantage cannot be utilized when crucibles with limited thermal shock resistance are used. Temperature control of induction-heated melts is poor, and the stirring effect increases the rate of contamination of the melt from the crucible, slag, or the furnace atmosphere; liquation and controlled solidification are difficult to carry out. Because of these objections, resistance heating was chosen. A 10 kw Globar resistance furnace of low heat capacity permitted uniform heating of a uranium charge to its melting point in 45 min. The furnace was insulated with a removable aluminum shield so that, after melting and removal of the shield, the furnace could be quickly cooled to room temperature. The furnace was equipped with an apparatus for directional solidification; see Fig. la. The crucible was suspended in the center of the furnace; and when the melting was complete, the crucible was slowly lowered into the cold end of the furnace tube. Solidification took place upward from the bottom; and when the rate of lowering was small, a sound ingot free from sink holes and shrinkage cavities was produced. To remove the large quantities of gas contained in the electrolytic crystals, melting in a high vacuum is mandatory. While, from the standpoint of contamination, melting in a highly purified argon atmosphere appeared feasible, lithium and potassium removal proved less efficient under such conditions. Also, a vacuum-melted ingot has a cleaner surface than one melted in an inert atmosphere. The vacuum system must be of very high pumping speed and leak tight so that a vacuum of less than 2x10-7 mm Hg is attainable when the system is pumped down cold. The system must have a high pumping speed, so that the pressure maximum which may rise to 1x10-4 mm during heating can be quickly reduced

Jan 1, 1956

By S. B. Christy

The fact that many millions of gold have been extracted by the cyanide process, during the last five or six years, from South African tailings which could not be profitably worked by any other method previously tried upon them, lends a peculiar practical interest to this branch' of metallurgy. Numerous writers have recently made valuable contributions on the process without exhausting the many complexities of the subject. Among the first American writers on the subject in its modern aspect were two former students of the University of California, Mr. Louis Janin, Jr., and Mr. Charles Butters. Young Janin was one of the first to enter this field, and performed much useful experimental work in the early stages of the history of the process. At about the same time, Mr. Charles Butters, who had left California to erect chlorination works for the Robinson mine at Johannesburg, became interested in the cyanide process, and, after getting the chlorination plant in working order, put up, for working the tailings from the Robinson mine, a cyanide plant which achieved the first large-scale success ever made with this process. The papers which Charles Butters, together with John E. Clennell and Edgar Smart, have contributed on the chemistry of the process, were among the first to give any adequate idea of its nature.* Another important contribution to the literature of the subject is the paper of Dr. A. Scheidell, published in 1894 as a " Bulletin of the California State Mining Bureau." This contains an admirable summary of the state of the art at the time of its publication.

Jan 1, 1897

By George Sachs, S. M. Clark, George Espey

he tendency of a commercially drawn cartridge case to crack in the mercury test and the relation of cracking tendency to residual stress retained after drawing were studied. The fourth drawpiece (next to the final) of caliber 0.30 cartridge cases produced by Frankford Arsenal were selected as test pieces. These exhibited an exceptionally high cracking tendency, making a detailed study possible. To obtain fast cracking in the mercury test, about 0.0015 to 0.003 in. must be removed from the wall thickness of the drawpiece by pickling, and it must be subjected to the mercury test immediately after washing. Removal of the adhering mercury by annealing and subsequent squeezing of the case in a vise was used to reveal definitely the presence or absence of cracks. Various lots of apparently identically fabricated cases were shown to possess a different cracking tendency. Machining off or boring a hole in the base gradually reduced and eventually eliminated the cracking tendency. On the contrary, shortening of the wall (body) reduced the cracking tendency only if the wall became so short that the cracking zone was directly affected. By boring out the base and pickling from the outside and then splitting the resulting rings, it was possible to determine the approximate stress distribution in the base and in the adjacent part of the wall. Small compression stresses were present in the core and the major part of the base, while the surface of the base and the adjacent wall contained high circumferential tensile stresses. On the contrary, the wall when parted from the base contained only insignificant residual stress. The conception is advanced, that the stress distribution in a drawn cartridge case corresponds fundamentally to that of a tube (wall) shrunk on a disk (base). Such a stress distribution results from the tendency of the base to recover elastically by an increase in diameter from the biaxial compression during drawing while the wall exhibits little tendency to change its diameter after progressing through the die. This is confirmed by measurements which show the base diameter to be slightly larger than the wall diameter.

Jan 1, 1945

By J. T. Norton, N. J. Grant, I. S., Servi

Coarse grained high purity aluminum was tested in creep at temperatures of 400° to 1200°F to develop subgrain structures. Measurements of subgrain size, distribution, and rotation were made from X-ray diffraction patterns. Subgrain size and distribution were checked metallographically and the size was compared with average slip band spacing. The slip family was determined for several specimens. THE interest and research recently evident abroad in the role of subgrain formation and polygon-ization as a contribution to the creep of metals at elevated temperatures is deserving of greater attention in this country. Such metallic subgrains can be defined as macroblocks existing within the grains. The general observation has been that the macro-blocks which belong to the same grain have a maximum difference in orientation of a few degrees. In spite of the considerable amount of work that has been done since Jenkins and Mellorl observed the "division of existing crystals into smaller units when deformation occurs at an annealing temperature," the subject of subgrain formation is only now receiving truly active discussion and investigation. The existence of subgrains has been revealed by metallographic methods, as in the work of Jenkins and Mellor,1 and by X-ray methods, first applied to this problem by Homes.' Hirst3 and Calnan and Burns4 applied the back-reflection Laue technique to the study of coarse grained specimens. Wood et al.5 and Greenough and Smith' examined the ring obtained with a back-reflection camera for the study of fine grained specimens. In addition to the above, the transmission technique was used by Wood.6 A special technique was developed by Guinier and Tennevin8 in order to improve the resolution. Metallographically, the subgrains have been observed directly on the surface of deformed specimens by Wood et al.,3 or have been made evident on repolished surfaces by applying a suitable etching reagent. The latter technique, first suggested by Lacombe and Beaujard,9 was then improved by Wyon and Crussard.10 Subgrains can be formed in single crystals after small amounts of bending followed by heating after this cold work, or during deformation at elevated temperatures. The first phenomenon was analyzed by Cahn11 for the simple case of pure bending followed by annealing. Cahn suggested a mechanism of subgrain formation based on the dislocation theory and called this phenomenon "polygonization." He extended this mechanism to the more complex case of local bending, such as the bending which may occur when a polycrystalline specimen is deformed in tension. Cahn's suggestion was later found quite consistent with the results obtained by Dunn and Daniels." An explanation has been presented recently regarding the formation of subgrains during deformation at elevated temperatures by Chang and Grant.'" In general, there are two schools of thought on the subject. One, according to Wood et al.,5 is that subgrain formation is a mechanism of deformation which is operative under certain conditions in the same way that the slip process is the mechanism of deformation which is operative under other conditions. The boundaries between the subgrains undergo a viscous flow which contributes substantially to the deformation of the material. The second, according to Cahn,13 Wyon and Crussard,10 and Chang and Grant,18 is that subgrain formation is the effect of simultaneous deformation and annealing and is,

Jan 1, 1953

By A. J. McEvily, R. C. Boettner, C. Laird

The processes leading to fatigue failure in the low-cycle range were studied to obtain an understanding of the basis of Coffin's law. Particular attention was paid to the manner of mack nucleation and to the determination of the portion of the total lifetime spent in crack propagation. It was observed that cracks are nucleated at surface notches meated during reversed plastic deformation, Principally at grain boundaries, and that crack growth occupies greater than 75 pct of the fatigue life. When inclusions are present, they are often the primary sites of crack initiation. From consideration of the incremental distances advanced by a crack in each cycle and of the lifetimes of different materials, it appears that the universality of Coffin's law arises from the similarity of crack-tip strain for a given applied strain amplitude, irrespecti7:e of material. STUDIES of low-cycle fatigue have been particularly rewarding in that a simple correlation between fatigue lifetime and plastic-strain range has been shown to exist. This empirical relationship takes the forml,2 Nner=C [1] where N is the number of cycles to failure, Er is the plastic-strain range defined as the total plastic strain per cycle (the sum of the tensile plastic strain plus the compressive plastic strain), n, the exponent, is a constant independent of the material to a first-order approximation and often has a value of about 0.5, and C is a constant which for a number of ductile and metallurgically stable materials is approximately 0.65 for fully reversed strain.3 This relationship has been shown to be valid for a wide variety of metals and alloys and is often referred to as Coffin's law. However, it is yet not clear why so many different metals and alloys exhibit the same over-all behavior in the low-cycle range. Less is known about the mechanisms of fatigue failure in the low-cycle range than in the high-cycle range, but it is expected that the processes would have much in common. For example, an important characteristic common to both high-and low-cycle ranges is that fatigue crack propagation can occupy a considerable portion of the total lifetime. This has been shown by Laird and smith4 by a count of the number of ripples present on the fracture surface of copper specimens, each ripple corresponding to one cycle of load. On the other hand, some marked differences have been noted. For example, in copper,5 nickel, and aluminum4 there is a greater tendency for grain boundary cracking to occur as the strain amplitude is increased. The purpose of the present work was to study further the processes leading to fatigue failure in the low-cycle range and to obtain an understanding of the basis for the validity of Coffin's law. Particular attention has been paid to the manner of crack initiation and to the determination of the portion of total lifetime spent in crack propagation. MATERIALS A number of metals and alloys were tested, although more attention was focused on a particular few, once general trends had become apparent. Alloys were selected so as to investigate the effects of crystal structure, number of phases, stacking-fault energy, and impurity content. The materials in this grouping were: high-purity copper OFHC copper 1100 aluminum (commercially pure) 70-30 brass (Cu-30 wt pct Zn)

Jan 1, 1965

By Raymond D. Sloan

Development and exploration in Oklahoma showed a definite increase in 1941 over 1940 in production, wildcat activity and total well completions. Geological and geophysical work continued and possibly increased slightly in amount. Oklahoma retained third place in the ranking of oil-producing states of the nation, topped only by Texas and California, and followed by Illinois in fourth position. Production averaged 416,800 bbl. daily, a 1.7 per cent increase, as compared with 409,900 bbl. daily for the year 1940. Maintenance of the state's relatively stable producing rate resulted from the discovery of numerous small pools, the recombing of old areas, the establishment of new producing horizons, and the drilling of an increased number of marginal wells. The market for the Mid-Continent crude was strengthened materially to meet the increased demand. Coincident with a deeline in production in Illinois, shipment of Oklahoma-Kansas crude to the eastern points averaged 453,000 bbl. per day, an increase of 49.4 per cent as compared with 1940. The movement south amounted to an average of 42,000 bbl. per day, a loss of 41.7 per cent. Secondary-recovery programs in Oklahoma were given more consideration, operators realizing that in the future many pools would necessarily have to resort to this type of operation. Five permits for water-flooding were issued by the Corporation Commission during the year. These projects were in Rogers, Wagoner and Nowata Counties, in the shallow northeastern area, which has relatively extensive development of this type in the Bartles-ville sand at from 600 to 1000 ft. in depth. Gas repressuring of an individual lease in the 35-year old Glenn pool, Creek County, proved relatively successful, and after a year's operation was extended to cover a much larger area, with several operators participating. More of this type of work is expected in the future; however, it was given an initial setback when the legislative proposal authorizing secondary recovery in the Wilcox zone of Oklahoma's largest pool, the Oklahoma City pool, was pigeonholed by the committee. A continuation of the low discovery rates within the state would possibly lead to a revival of interest in the project. Many pools formerly classified as prorated areas were removed from this classification and transferred into the group of settled production. At the close of the year the issuance of the Federal Conservation Order M-68 and the interrelated Preference Rating Order P-98 caused a sharp decline in drilling operations, which is expected to continue until such operations are stabilized at a lower rate. The ultimate effect of these two orders on discoveries, production and reserves is a matter of speculation and conjecture. During the year, 2110 new wells were drilled, an increase of approximately 18 per cent as compared with the previous year. Of the total, 1235 were oil wells with a combined initial potential of 342,754 bbl. daily, 178 were gas wells with a total

Jan 1, 1942

By H. I. Aaronson, H. A. Domian

The self-diffusivity of Ag10 has been measured as a function of temperature and composition in AgMg. a CsCl-type intermetallic compound with a substitutional defect structure on both sides of the stoichiometric (50 at. pct Mg) composition. These measurements show that In D increases linearly, and both In Do and Q decrease linearly with deviation from stoichiometry. The slopes of these lines are significantly steeper in magnesium-rich alloys. Equations for the variation of Q with composition have been derived by application of the theory of random walk processes on the assumption that diffusion in compounds of this type takes place by the six-jump cycle mechanism of Huntington, Elcock, and McCombie. The favorable agreement obtained with experiment furnishes fresh support for the correctness of this assumption. A principal result of this treatment is that. although the concentration of vacancies is considerably higher in the silver sublattice than in the magnesium sublattice, the acfivation energies for movement of the magnesium sublattice vacancies are so much lower that these vacancies are responsible for effectively all diffusion of silver in this compound. A tendency for vacancies of both types to be kinetically bound to wrong atoms is also noted. THIS study was undertaken to examine the influence of substitutional defects upon self-diffusion in an intermetallic compound, AgMg, with a CsCl-type crystal structure. The CsCl structure is exception- ally simple. At the equiatomic or stoichiometric composition in a binary alloy, it consists of two interpenetrating simple cubic sublattices, each of which is exclusively populated by the atoms of one species. When atomic size and other factors are favorable, deviations from stoichiometry can be entirely accommodated by the substitution of atoms of the species present in excess of 50 at. pct on the sublattice of the other species on a one-for-one basis. Under this condition, the only vacancies present are those formed by thermal activation. The excess atoms thus incorporated into the sublattice of the minority species may be considered as substitutional defects in this sublattice. Several X-ray studies have shown that the defect structure of AgMg is entirely of the substitutional type on both sides of the stoichiometric composition.1"3 The thermodynamic investigation of Kachi indicates that, aside from a low level of thermal disorder and these constitutional defects, order is maintained to the solidus temperature. This compound is therefore a particularly useful vehicle for a study of the influence of substitutional defects upon diffusion kinetics. Other advantages of AgMg for this purpose include: the broad composition region, as much as approximately 10 at. pct on either side of the stoichiometric (50 at. pct Mg), in which the compound is stable; the comparatively low temperature range of the solidus (820°C and below),5 making diffusion anneals near this range experimentally convenient; the reasonably good machinability of the compound, permitting utilization of the standard sectioning method of radiotracer analysis; and the availability of a good tracer, A for one of the constituent species. While this investigation was in progress, Hagel and westbrooks reported data on the self-diffusion

Jan 1, 1964

By F. T. Selleck, H. H. Reamer, B. H. Sage

An experimental investigation was made of the effect of temperature upon the three-phase pressure associated with the propane-water and propene-water systems when hydrates were present. In addition, the characteristics of the propane-propene-water system were established over a limited range of ternperatureo under conditions such that hydrate was formed. The hydrate phase for this system may he a solid solution and the distribution of propane and propene in it is similar to that found in the coexisting hvdrocarhon liquid phase. INTRODUCTION A knowledge of the characteristics of hydrates of the hydrocarborrs encountered in industrial practice is of importance in connection with the design of process equipment. Villardl.1,2 carried out early studies of hydrates, and de Forcrand1 con-sidered the more probable compositions of the hydrates of hydrocarbons. Hammerschnid1 presented information about the propane-water and the isobutane-water systems. Scheffer5 studied the hydrate of hydrogen sulfide in detail, and de For-crand reported on the hydrates of krypton, argon, and xenon.1 Roberts and co-workers1,2 determined the nature of the hydrates formed in the methane-water and ethane-water systems. Carson and Katz10 studied the methane-propane-water, methane-pentane-water, and the methane-hexane-water systems in the four-phase region. The results of this rather extensive investigation indicated that the paraffinic hydrates formed solid solutions. The experimental evidence now available does not Support the existence of hydrates of the pentanes-antl-heavier hydrocarhons but it cannot be stated with certainty that such hydrates are not formed. Stackelherg. 11,12,13 made extensive studies of the crystal structure of paraffinic hydrate; by means of x-ray techniques and found that hydrates poses; a definite structure and composition. The existence of such a Structure does not preclude the firmation of Solid solutions of hydrates in aqueous systems containing two or more hydro-carbon~. Wilcox, Carson and Katz" reviewrd the information on the hydrates of importance in the processing of natural gas and presented data concerning their formation from natural gas. Kobayashi and Katz1' made studies at high pressure of the Hydrate of methane. and Unruh and Katz"' investigated hy-drates in mixtures of carbon rlioxide and methane. Frost and Deaton contributed to the knowledge of the composition of the paraffinic hydrates The irregularities in the experimental results were several times the expected uncertainties. This experience confirms the behavior encountered by other investigators indicating that hydrates tend to occlude water during their formation, thus rendering difficult the direct measoremeut of their composition. Miller and Strong2 investigated a number. of paraffinic hydrates from the standpoint of their possible application to (, the industrial storage of gas. Powel1 studied the effect of solutes upon the decomposition temperature of paraffin hydrates. Marked lowering of the decomposition temperature at a given pressure may he obtained by the use of such additive agents as ethylene glycol, urea. and sodium chloride. APPARATUS AND METHODS Two method* were here employed to study the behavior of hydrates. The first involved a glass capillary within which the hydrocarbons and water were confined over mercury. The second made use of a double-ended weighing bomb technique." The glass capillary equipment has been described elsewhere.'" A schematic drawing of it is presented in Fig. 1, where the arrangement of the agitator and mercury reservoir is shown in some detail. The lower part of the glass capillary, D, was enlarged to afford space within which the fluids used in the investigation could he stored at low pressures after their introduction through the valve. G. The temperature of the capillary was controlled by the circulation of a hydrocarbon oil of low viscosity from the agitated bath, B, through the vacuum jacketed column. C. The pump, A, was employed for the circulation of this oil. A relatively clear view of the capillary tube, D, was obtained through the vacuum jacket. Mercury was introduced into the lower part of the vessel, E, from

Jan 1, 1952

By J. B. Newkirk, W. G. Martin

Oxidized cobalt powder is known to have a magnetic hysteresis loop which is asymmetric with respect to the magnetization axis. The experiment described herein shows that the orientation relationship between the basal plane of hexagonal cobalt and the oxide which forms upon it at 400°C is {111}ux//{100.1 }co <110>ux//<11.O> This orientation relationship allows a magnetic interaction between the antiferromagnetic oxide and the ferromagnetic substrate which could account for the offset hysteresis loop. Oxidized nickel powder has a symmetrical hysteresis loop and so is apparently not influenced by any magnetic interaction between metal and oxide. The orientation of the oxide (cubic) was found to be identical with that of the nickel substrate when the oxide forms on a polished surface parallel with {111} Ni. IN 1956 W. H. Meiklejohn and C. P. Bean discovered that fine particles of cobalt which had been prepared in a certain way have a magnetic hysteresis loop which in a strong field is asymmetric relative to the magnetization axis.&apos; The cobalt powder exhibited this unusual magnetic property only after it had been oxidized in air or oxygen; it lost the shifted hysteresis loop when the oxide was reduced in hydrogen. X-ray and neutron diffraction&apos; experiments showed the presence of cobaltous oxide (COO) and hexagonal cobalt in samples exhibiting the biased hysteresis loop and specifically showed no indication of any other compound with the exception of mercuric oxide.* The magnetic hysteresis loop becomes symmetrical above the Nee1 temperature (paramagnetic state) of COO. Therefore, it was concluded that the anomalous magnetic behavior is associated with the influence of cobaltous oxide upon the metallic cobalt. It has been proposed that crystallographic coherency may exist between the cobalt and a plane of some antiferromagnetic material which has unbalanced spin distribution and sufficient magnetic anisotropy to hold its spin in the direction which existed when the specimen was cooled. COO has these properties. Therefore, Roth&apos; has suggested that cobaltous oxide may form with a {111} plane parallel and coherent with the basal plane of the hexagonal cobalt metal and proposed that, as consequence of the antiferromagnetic interaction between COO and the underlying cobalt, the magnetization direction in oxidized fine Co particles may be ro-lated from the easy c-direction.2 Such a relationship, he proposed, would explain the observed magnetic effect in oxidized cobalt powder. The main purpose of this study was to determine the orientation relationship, if any, between the basal plane of cobalt and the oxide which forms upon it. Attempts to produce a film of COO which was strong enough to be handled were not successful. However we did succeed in making a film of CoCo2O, which was strong enough to be removed from the cobalt substrate and mounted on an electron-microscope grid. Because of the close structural similarity of COO and CoCo2O, we believe the orientation relation found for CoCo2O, on cobalt probably also holds for COO on cobalt. The epitaxial relationship of NiO and Ni also was investigated. To date no shifted hysteresis loop has been observed with nickel powder. However, the similarity of atomic array in cobalt and nickel leads to the prediction that a {111} of NiO may be parallel with a (111} of nickel. Experimental Method Cobalt-Cobalt Oxide—A coarse-grained specimen of a (hexagonal) cobalt was prepared by allowing a large crystal of fee cobalt to transform slowly at 400°C. The crystal was then cut to expose a surface parallel with the basal plane. A back reflection Laue X-ray photograph showed that the 00.1 plane was within 2" of the cut surface. The surface was mechanically polished and then electro polished in 85 pet orthophosphoric acid after which the crystal was held for 30 min at 400°C in air. During this heat-treatment the surface darkened slightly due to the oxide film which formed. The film was not thick enough to give an X-ray diffraction pattern, even by a glancing-angle technique. Glancing-angle electron diffraction was not possible either, owing to the interference of the electron beam with the high magnetic fields which exist at the 00.1 surface of the cobalt. However, it was possible to make an electron-diffraction photograph of the oxide film by stripping it from the cobalt substrate using the method described later. By maintaining reference marks carefully, it was possible to preserve the orientation relationship between the stripped film and the substrate on which it was formed. The oxidized surface of the crystal was first covered with a 1 pet solution of collodion (cellulose nitrate) in amyl acetate. When the film was dry, small rectangles were scored on the surface with a needle point. The specimen was then repolished

Jan 1, 1959