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By B. Heide, A. Bergrnann

The Meggen mine and the concentrator plant of the Sachtleben Bergbau GmbH are located in the southern part of the Ruhr district of the Federal Republic of Germany. The mine has been in operation for more than 100 years, but the concentrator described in this paper was started up in January 1963. The Meggen orebody is of sedimentary origin and occurs in a zone of limestones, graywacke and shales of Devonian age. The average thickness of the deposit is 3 meters and due to an intense folding of the area, the mineralized zone dips steeply at 80º towards the north.

Jan 6, 1973

By Charles Clayton

CAST-STEEL runners, while not interesting from a commercial standpoint, furnish valuable material for microscopic study. Foley1 found not only the usual ingot structure, but zones of Widmannstattian structure, which he explains as due to differential crystallization. The writer, in examining nickel-steel runners, found a type of pro-eutectoid ferrite that is unusual and most probably new. The runner in question was 8.75 cm. (3.5 in.) in diameter and analyzed at its center 2.69 per cent, nickel and 0.350 per cent. carbon and at its edge 2.62 per cent. nickel and 0.359 per cent. carbon. The macrostructure, which is the usual type, is shown in Figs. 1 and 2, which are a cross-section and the longitudinal surface, respectively. Slight segregation of ferrite can be seen near the center of the segment and at other points near the edges of polyhedral grains. Stead's reagent brings out the dendritic structure within the grains as shown in Figs. 3 and 4. This texture is what would be expected of such a steel. Figs. 5 to 10 show the peculiar swirls of pro-eutectoid ferrite, the finding of which prompted this paper. These swirls, or eddies, if such a term can be applied, occur in all parts of- the runner and in all parts of the individual grains. I he tipper left-hand figure shows this ferrite at a grain boundary; the middle left-hand figure shows the inner portion of a grain; and the lower left-hand figure shows these swirls at the edge of a grain which is also the outer edge of the runner. Straight-lined ferrite associated with swirls is found in the areas of Figs. 11 and 12. The texture of the carbon-bearing constituent of the runner is shown to- some extent in Fig. 12, the pearlite being very fine or sorbitic. Higher magnification does not bring out any new features either in the peculiar ferrite or in the pearlite. Figs. 13 and 14, at 240 diameters, show the curved and straight-lined ferrite.

Jan 3, 1920

By Charles Y. Clayton

Cast-steel runners, while not interesting from a commercial standpoint, furnish valuable material for microscopic study. Folcyl found not only the usual ingot structure, but zones of Widmannstättian structure, which he explains as due to differential crystallization. The writer, in examining nickel-steel runners, found a type of pro-eutectoid ferrite that is unusual and most probably new. The runner in question was 8.75 cm. (3.5 in.) in diameter and analyzed at its center 2.69 per cent. nickel and 0.350 per cent. carbe a and at its edge 2.62 per cent. nickel and 0.359 per cent. carbon. Th macrostruc-ture, which is the usual type, is shown in Figs. 1 and 2, which are a cross-section and the longitudinal surface, respectively. Slight segregat'ion of ferrite can be seen near the center of the segment and at other points near the edges of polyhedral grains. Stead's reagent brings out the dendritic structure within the grains as shown in Figs. 3 and 4. This texture is what would be expected of such a steel. Figs. 5 to 10 show the peculiar swirls of pro-eutectoid ferrite, the finding of which prompted this paper. These swirls, or eddies, if such a term can be applied, occur in all parts of the runner and in all parts of the individual grains. The upper left-hand figure shows this ferrite at a grain boundary; the middle left-hand figure shows the inner portion of a grain; and the lower left-hand figure shows these swirls at the edge of a grain which is also the outer edge of the runner. Straight-lined ferrite associated with swirls is found in the areas of Figs. 11 and 12. The texture of the carbon-bearing constituent of the runner is shown to some extent in Fig. 12, the pearlite being very fine or sorbitic. Higher magnification does not bring out any new features either in the peculiar ferrite or in the pearlite. Figs. 13 and 14, at 240 diameters, show the curved and straight-lined ferrite.

Jan 1, 1922

By Charles Y. Clayton

Cast-steel runners, while not interesting from a commercial standpoint, furnish valuable material for microscopic study. Folcyl found not only the usual ingot structure, but zones of Widmannstättian structure, which he explains as due to differential crystallization. The writer, in examining nickel-steel runners, found a type of pro-eutectoid ferrite that is unusual and most probably new. The runner in question was 8.75 cm. (3.5 in.) in diameter and analyzed at its center 2.69 per cent. nickel and 0.350 per cent. carbe a and at its edge 2.62 per cent. nickel and 0.359 per cent. carbon. Th macrostruc-ture, which is the usual type, is shown in Figs. 1 and 2, which are a cross-section and the longitudinal surface, respectively. Slight segregat'ion of ferrite can be seen near the center of the segment and at other points near the edges of polyhedral grains. Stead's reagent brings out the dendritic structure within the grains as shown in Figs. 3 and 4. This texture is what would be expected of such a steel. Figs. 5 to 10 show the peculiar swirls of pro-eutectoid ferrite, the finding of which prompted this paper. These swirls, or eddies, if such a term can be applied, occur in all parts of the runner and in all parts of the individual grains. The upper left-hand figure shows this ferrite at a grain boundary; the middle left-hand figure shows the inner portion of a grain; and the lower left-hand figure shows these swirls at the edge of a grain which is also the outer edge of the runner. Straight-lined ferrite associated with swirls is found in the areas of Figs. 11 and 12. The texture of the carbon-bearing constituent of the runner is shown to some extent in Fig. 12, the pearlite being very fine or sorbitic. Higher magnification does not bring out any new features either in the peculiar ferrite or in the pearlite. Figs. 13 and 14, at 240 diameters, show the curved and straight-lined ferrite.

Jan 1, 1922

By Frank J. Windolph

Grinding Practice-These tests were run in the 9 ft diam by 8 ft long grate discharge ball mills at Climax. Each mill functions in closed circuit with a 78 in. Akins duplex high-weir classifier, and a circulating load of 300 pct is maintained. The size of the mill feed is 6 pct on 3/8ths, which is ground to pass 28 mesh. Testing Methods-Each grinding section is equipped with a conveyor scale on the ball mill feeder belt, a watt-hour meter on the ball mill motor, and an automatic sampler for the ground product. These instruments are exceptionally valuable to the mill testing program.

Aug 1, 1956

By D. W. Smith

THE beta solid solution phases of the systems copper-zinc, copper-aluminum, copper-tin and silver-zinc are structurally analogous.1 R. F. Mehl and 0. T. Marzke2 have shown that the a phase upon segregating from the 0 phase in the system copper-zinc takes the form of needles lying parallel to a [111.] direction or some similar direction, such as [556], of the parent solid solution, and that the a phase upon segregating from the ß phase in the system copper-aluminum also takes the form of needles. By analogy they assume that in this case also the segregate needles lie parallel to the [111] or [556] direction in the ß lattice. The purpose of this investigation is to determine whether the structures resulting from segregation of the a phases from the respective 0 phases of the systems copper-tin and silver-zinc are analogous to those obtained by Mehl and Marzke in the systems copper-zinc and copper-aluminum.

Jan 1, 1932

By F. V. Lenel, M. V. Rose, A. B. Backensto

WHEN aluminum-flake powders are compacted and hot pressed and the resulting compacts are extruded or hot forged, a group of materials with unique properties is obtained. Not only do they exhibit high room-temperature strength of the order of some of the aluminum alloys, but they maintain this strength even after prolonged heat treatment at temperatures up to 900°F. Moreover, their strength decreases much less with increasing temperature than that of aluminum alloys of comparable room-temperature properties. Irmann,'" who discovered and first described this group of materials, which was called SAP, showed that the room-temperature mechanical properties of the extrusions are a function of the oxide content of the powders and therefore the oxide content of the extrusions. The higher the oxide content, the higher are their tensile strength, yield strength, and hardness, and the lower their ductility. Lyle" investigated the relationship between mechanical properties at elevated temperature and oxide content in the course of the development work of the Aluminum Co. of America on materials, called APMP, similar to those developed in Switzerland. He found that at 600 °F, just as at room temperatures, tensile strength and yield strength increase and elongation decreases with oxide content. A careful study of his data (Fig. 3, loc. cit.) shows, however, that the scatter is more pronounced than at room temperature. Gregory and Grant's data on the creep5 and stress-ruptureb roperties of the one commercial grade of the Swiss SAP and the various grades of APMP indicate that creep strength and stress to rupture also generally increase with increasing oxide .content. Ever since this new group of materials was discovered, attempts have been made to explain the mechanism by which they obtain their high room-temperature and particularly their elevated-temperature strength. In most of the attempts the new material was considered as a dispersion of aluminum oxide particles in a matrix of aluminum. Ir-mann, Von Zeerleder, and Rohner' applied a theory on dispersion strengthening developed by Rohners to the flake-powder extrusions. According to this theory the elastic limit S, of a dispersion would depend upon the average distance between the dispersed particles L according to the equation: 2 E ¦ a where E is the modulus of elasticity and a the distance between nearest neighbors in the lattice of the matrix material. Irmann and co-workers assumed

Jan 1, 1958

By E. R. Shorey

FLOTATION-Mill operator's have recognized that slimes are detri-mental to the flotation concentration of zinc ores. The, presence of primary slime in many of the Wisconsin ores is largely responsible for the failures experienced in treating these ores by flotation. These failures have discouraged the adoption-of the flotation process by opera-tors in the Wisconsin zinc district. The removal of slimes by decantation seemed to be the obvious way to meet the problem of treating slimy or' clayey ores by flotation. To facilitate the removal of slime, it was decided to mix the ore pulp with sodium silicate, which acts to deflocculate the pulp.1 Deflocculation causes slime suspension, making it possible to separate the slime from the sands by decantation.2 Since the literature contains little definite information on the use of sodium silicate to deflocculate ore pulps, a series of tests was conducted to obtain the necessary information. Tests to determine the settling rates of sand and slime in deflocculated pulps were conducted on a dolomite-marcasite-sphalerite ore ground to minus 80 mesh (175 microns) and mixed with water to form a pulp. The deflocculator3 was Mallinckrodt 40° to 42.5° Bé. liquid sodium silicate (Na20 + 3.25Si02). .By microscopic analysis the suspended slimes4 were found to be minus 15 microns (approximately 1000 mesh).

Jan 1, 1934

By Kidd, Robert L.

INASMUCH as galena and sphalerite flotation concentrates are being produced that contain over 95 per cent galena or sphalerite, it is not unreasonable to believe that a flotation concentrate assaying at least 80 per cent of native gold can he secured provided the gold is free. As yet, little if any fundamental information has been published concerning the flotation of free gold either alone or in the presence of sulfides. So far, we are unable to make as complete a separation of gold from sulfide minerals by flotation as is possible in, the separation of one sulfide from another by this method. An introductory study of the flotation of several free gold ores has been made in our Utah laboratories. For this study three general types of gold ores were chosen, namely: (1) Quartzite containing 0.26 oz. gold per ton in which no base metals are present; (2) sulfide ore (2.04 oz. Au; 1.31 oz. AO containing pyrite as the only sulfide present and the gold free; and (3) oxidized ore (1.10 oz. Au; 0.70 oz. Ag) from an oxidized zone of the vein from which sulfide ore (No. 2) was taken; little sulfide iron was present.

Jan 1, 1932

By Charles H. Jones

Jan 1, 1905

By K. E. Brown, F. W. Jessen

By utilizing an 8,000-ft experimental field well equipped with 10 gas-lift valves and 10 Maihak pressure recorders, gas-lift tests were conducted with port sizes ranging from 5/16 through I in. The well was equipped to provide accurate means of measuring surface pressures, temperatures, quantity of injection gas and fluid production. The tests were conducted in 2%-in. OD tubing, and the well was making 95 per cent water. A complete evaluation of gas-lift-valve port sizes shows the relationship of per cent recovery, gas-liquid ratios, minimum pressure created at the operating valve and horsepower requirements for each port. The length of time necessary for the fluid in the tubing to reach equilib.rium conditions after each cycle was recorded. Fallback of fluid at depths of 477, 969, 1,685, 2,493 and 4,290 ft was noted. For each port size, pressure loads of 2.50, 300, 350, 400 and 450 psi were lifted with a valve operating at approximately 550 psi at 6,000 ft. Gas-liquid ratios for each load were varied from excess gas to a gas volume per cycle whereby the load failed to reach the surface. Numerous curves are presented in evaluating the accumulated dara. The results show a 1-in. port to be the most efficient under all conditions. The production of intermittent liquid slugs against different-sized surface chokes was evaluated. These tests were conducted from a 7/16-in. ported valve at 4,072 ft. Tests indicate that, when possible, a %-in. in diameter choke or larger should be used at the surface. In the past few years most of the advancement in gas-lift operations has been made in continuous-flow operations. Yet, it is estimated that at least 70 per cent of the wells on gas lift in the United States are of the intermittent type. Since the term "slug flow" is sometimes used in both intermittent- and continuous-flow operations, it would be well to distinguish between the two types of flow. Continuous-flow gas lift is defined as a method whereby the fluids are produced at a continuous rate at the surface. This generally requires a continuous injection of gas through a surface choke; however, various other control devices sometimes are installed to eliminate freezing, to shut-off gas during natural flow periods, etc. The actual flow of fluids in the tubing may be of the slug type (one of many flow patterns known to exist in continuous flow). Intermittent flow is defined as a method of gas lift whereby the liquid is produced in separate piston-type slugs. Perhaps this type of flow could best be thought of as a ballistic-type flow where the liquid leaves bottom as a piston, propelled by a slug of expanding gas. Gas generally is injected through some type of control at the surface at predetermined intervals. However, the valve may have characteristics whereby gas can be injected through a small choke and still result in a ballistic-type flow. The purpose of the experimental work was to evaluate the most efficient port size to be used on the operating valve for the ballistic type of lift and, in addition, to establish the importance of utilizing a surface choke large enough to allow slugs to be produced without detrimental effects. This work is part of a compre- hensive study of both intermittent-and continuous-flow gas lift, representing a joint project conducted by the Ohio Oil Co., the Sun Oil Co., Otis Engineering Corp, and The U. of Texas. The problem of evaluating port sizes has been given little previous attention. Some work undoubtedly has been done which has not been published to date. Some tests were conducted when the wireline, mechanically-opened valve (Nixon) first came on the market. This valve was capable of utilizing full tubing area as its port size. It is known that this was a very efficient valve, but to the authors' knowledge the results of tests have never been published. EXPERIMENTAL EQUIPMENT These tests were conducted on an actual field well, the Ohio-Sun Unit Well No. 2-E, in the North Markham-North Bay City field, Matagorda County, Tex. The well incorporated 23/8-in. OD tubing and produced 95 per cent water. Since the running of equipment was to be quite elaborate and expensive, a well was selected in which both intermittent- and continuous-flow tests could be conducted. This particular well was capable of producing in excess of 1,000 B/D of liquid (95 per cent salt water), yet with a 3/64-in. in diameter bottom-hole choke, production was controlled to 82 B/D. Most of the intermittent tests were conducted at this low rate. Figs. 1 and 2 show all the surface and down-hole equipment. As can be seen, every attempt was made to insure that ample equipment was available for reliable testing procedures. Fig. 1 shows the surface testing equipment. The input gas was controlled first by a regulator, then

By Gilbert P. Moore

Petroleum operations in Bolivia are still limited to those of the subsidiaries of the Standard Oil Co. of New Jersey. Development work is being carried on at Sanandita and at Bermejo and testing operations in the north. Five wells have been completed at Sanandita. Wells 1 and 2 are producers, 3 and 5, which are north of 1 and 2, are poor wells, and well 4, to the south, was dry. In the Bermejo field, well 5 has just been completed. No information as to the production is obtainable. In the north one string was operated at each of the following locations: Machareti, Camatindi and Camiri. The well completed at Machareti during the year was a failure. The result of the others is not known. It is reported on good authority that a pipe line will be completed in 1931 to connect the Sanandita field with the Lomitas field in the Argentine. This will place Bolivia among the ranks of the producing countries of South America for the first time. This development indicates that some arrangement has been arrived at with the Argentine Government for the importation of Bolivian oil. During 1930 the Bolivian Government declared in effect the new Petroleum Law which had been expected for such a long time. One of the first acts of the military junta, which rose to power through a coup d'état, was to cancel this law, so that Bolivian oil operations are still under the old law of 1921. One new local company was formed to exploit 1,500,000 hectares near the town of Cochabamba. The Bolivia Concessions, Ltd., which had a concession permitting the selection of 17,000,000 acres in eastern Bolivia, is reported to have failed in 1930 and is now being liquidated. Chile During 1930 the Chilean Government entered into a contract with an individual to explore in five distinct zones of the Republic. According to the contract, geologists must be at work there by May 1 of this year and a well must be started by the end of 1931. If the operations are

Jan 1, 1931

By F. E. Bachman

There is such a great variety of opinion concerning the best method of determining phosphorus in pig iron and steel, that a list of determinations, on a uniform sample of pig iron, together with a short description of the methods used by different chemists, and a few experiments on the accuracy of some of the methods used, [nay be of interest to members of the Institute. All the results given in List A are from the same lot of drillings, thoroughly mixed, except Nos. 8 and 9, and 28 to 32 inclusive, which are from the same pig, but were taken at a later period.

Jan 1, 1882

By R. P. Carreker, J. C. Fisher

Cheep tests are normally constant load tests. Such tests approximate some types of service conditions and therefore are justified from the engineering point of view. Coupled with this consideration is the advantage of simplicity inherent in constant load tests, as contrasted with the comparatively complex requirements of a constant stress test. It is not surprising that the vast majority of creep tests reported are of the constant load type. Despite the enormous amount of accumulated creep test data, plastic flow is by no means completely understood. The widespread use of constant load tests is at least partly responsible for this lack of understanding. Any attempt to analyze deformation must involve the more fundamental quantity stress, rather than load. It is possible to predict constant load behavior from known constant stress data, but the reverse is much more difficult. When a metal specimen elongates, as in a creep test, the cross section decreases, maintaining constant volume. Thus For a constant stress test the force on the specimen must be decreased as the cross section decreases, that is, this force must be inversely proportional to the elongation of the specimen. An-drade has described three methods of obtaining the constant stress condition,l-3 each of which is relatively complex. The most recent proposal,³ suggests a major simplification which maintains the simplicity of the constant load test while approximating quite closely the desirable condition of constant stress. Andrade's device is admittedly more accurate but the method described below has definite advantages Consider a specimen in the form of a "V" supported at its ends. If a weight be applied at the vertex of the angle, the stress in each leg of the "V" If this stress causes an elongation ?1 in each leg of the "V," the angle decreases from a. to a smaller angle a1. The quantity sec — thus decreases with specimen elongation while the quantity 1/A increases. By selecting proper initial conditions it should be possible to hold S/So very nearly constant at unity. The proper initial conditions are realized when a0 is made equal to approximately 90°. Fig 1 compares the ratios of S/S0 for a0 = 85, 90, 95, 100°, with a0 = 0, that is, a straight speci- men, for true strains up to e = 0.10. It may prove convenient to measure X, the movement of the vertex, rather than the true elongation 1. Contour lines of X/lo are also plotted in Fig 1. The method for obtaining constant stress described above is especially suited to the testing of small wires, but may easily be extended to rods of any diameter through the use of a suitable grip which serves as the vertex joining two identical rods forming the legs of the "V." References 1. E. N. da C. Andrade: On the Viscous Flow in Metals, and Allied Phenomena. Proc. Roy. Soc., A, 84, 1, (1910-11). 2. E. N. da C. Andrade and B. Chalmers: The Resistivity of Polycrystalline Wires in Relation to Plastic Deformation, and the Mechanism of Plastic Flow. Proc. Roy. Soc., A, 138, 348, (1932). 3. E. N. da C. Andrade: A New Device for Maintaining Constant Stress in a Rod Undergoing Plastic Extension. Proc. Phys. Soc., 60, (3). 304, (March, 1948).

Jan 1, 1950

By J. B. Clark, A. S. Yue

The zone-melting technique can be adapted for the de-termination of the eutectic composition in complex metal systerrzs. The application of this method is demonstrated in a simple eutectic system, Mg-AE, in which the eutectic composition is known and in a complex ternary system, Mg-Al-Zn, in which the literature is uncertain as to the composition of the ternary eutectic. The advantages and limitations of this unique approach for the determirution of the eutectic composition are discussed. ThE eutectic composition in phase diagrams is usually determined by thermal analysis of a series of arbitarily selected alloy compositions. The temperatures of the liquidus and eutectic arrests for each alloy are plotted and the eutectic composition is estimated by extrapolation to the entectic temperature of the curve formed by the liquidus arrest temperatures for the series of alloys. Although this approach readily yields the eutectic temperatures, several dekrminations are needed to estimate the eutectic composition, even in a simple system. In a complex ternary system, a great many determinations are often necessary to estimate, even approximately, the ternary eutectic composition. Thus, the conventional method is inherently tedious and time consuming. The application of zone melting provides a relatively efficient method of determining the eutectic composition.' As an illustration, consider the zone melting of an alloy composition C, in the simple eutectic system A-B, shown in Fig. 1, under the ideal conditions of infinitely rapid diffusion in the liquid, no diffusion in the solid, and ease of nucleation of both phases. As the zone moves along the bar, the composition of the zone is enriched by solute rejected during the freezing of the a phase and the zone composition approaches the eutectic composition CE.Once the zone composition attains the lowest melting composition, i.e., the eutectic composition, it remains at this composition as the zone moves along the bar and finally freezes as such at the end of the bar. Chemical analysis of the end of such a zone-melted bar then should yield the eutectic composition CE of the system A-B. A corresponding analysis can be made for a ternary eutectic system. Under the ideal conditions noted above, only one pass of the molten zone is required to yield the eutectic composition. Experimentally, however, a solute-rich layer forms at the solid-liquid interface2 and the composition of the zone does not attain the eutectic composition as rapidly or as uniformly as in the ideal case outlined above. But with agitation of the melt, the ideal conditions can be approximated experimentally. Also, as shown below, zone melting permits a cumulative build-up of the solute at the end of the bar to the eutectic composition. The purpose of this paper is to demonstrate this unique method for determining the eutectic composition. The method is here applied to two systems: first, to the binary Mg-A1 system, in which the composition is well established, and second, to the complex Mg-Al-Zn system in which there is doubt concerning the composition of the ternary eutectic. EXPERIMENTAL PROCEDURE The zone-melting apparatus used in this study is described in detail elsewhere.3 Briefly, the binary alloy rods (5/8 in. in diam and 9 in. long) and the ternary alloy rods (5/8 in. in diam and 6 in. long), with the compositions given in Table I, were zone

Jan 1, 1962

By L. W. Emery

Undergrorlnd combustion operations were initiated in a 60-acre Bartlesville sand "shoe-string" reservoir in Allen Connty, Kans., in 1956. Tests in separate patterns were conducted using various co~nbinations of air and recycle gas to propagate combustion fronts from the injection toward the producing wells. These patterns were made up of 6 injection and 20 prodrrcing wells Gas and liquid prorluctiorz from each pattern was measured on an individual-well basis, and comparisons were made between the three patterns to ascertain the relative effects of injected gas composition on production behavior. Breakthrough of the combustion front at a well was characterized by an increase in water production from the well followed by an increase in bottomhole temperatrrre to approximately 250" F. After burning fronts had broken through at five producing wells, operations were terminated in 1960. From the total project approximately 79,000 bbl of oil were produced during thermal operations at a cumulative produced GOR of 23 Mcf/bbl. No appreciable change in the character of the produced crude was observed. Combustion in the reservoir was maintained with injected gas compositions ranging fronz 6 per cent oxygen in recycle gas to 100 per cent air. lnjectiotz of large quantities of recycle gas resulted in higher producing GOR's from offset wells than were measured from a pattern into ~vhich straight air ~vas injected. The air required to move the combustion front through I acre-ft of reservoir was computed to be 20 MMscf. This valrre was found to be relatively independent of the quantities of recycle gas injected. The recovery efficiency from the swept area was esti~izated to be about 59 per cent. Areas swept were similar in shape to tlzose obtained with a laboratory potentiometric model. Samples of sund taken from behind the burning front by coring indicated almost total oil removal from the sand. Petrographic analysis of the core samples indicated that the sand had been heated to peuk temperature of rlbout 1,200" F. No rignificant difference in peak temperature was forrnd in two areas where compositions of injected gas were quite different. Compression costs for thermal recovery were estimated to be $1,20/bhl of produced oil. INTRODUCTION The use of the "forward combustion" process as an oil recovery method has received a great deal of attention. This method involves ignition of the formation in an injection well, followed by propagation of a combustion front through the reservoir. Combustion is maintained by the injection of an oxygen-containing gas to react with reservoir hydrocarbons. As the flame front progresses through the reservoir, oil and formation water are vaporized, driven forward in the gaseous phase and recondensed in the cooler part of the formation. In turn, the condensed fluids push oil into the producing wellbores. Completed field tests of the process were first reported by Kuhn and Koch,' and by Grant and Szasz.' Results from other tests have since been reported by Walter,3 by Moss, White and McNeil,' and by Gates and Ramey." ach of these tests essentially utilized a single injection well surrounded by four or more producing wells. Sinclair Research, Inc., elected to do field experimental work using a number of test patterns in a single field in order that comparisons between various operating schemes could be made. The site selected and purchased in 1955 for this experimental work was a 60-acre Bartlesville sand reservoir located in Allen County, Kans. Combustion operations were initiated in mid-1956. Between that time and termination of the project in mid-1960, combustion fronts were propagated from injection wells to producers in three separate well patterns, using different mixtures of air and recycle gas. The test was terminated before sweep of the three patterns was complete so that information about the effect of combustion on the swept areas could be obtained by coring. Results from the test in the form of injection and producing well performance have been carefully recorded, and these form the general basis for this paper. DESCRIPTION OF RESERVOIR The reservoir in which the combustion tests were conducted is a Bartlesville sand "shoe-string", typical of a number of small reservoirs in Southeastern Kansas. Average reservoir characteristics are shown in Table 1. Fig. 1 is an isopachous map of the producing sand showing the reservoir to be approximately 400-ft wide and 2,500-ft long. Maximum net productive sand thickness is 21 ft. Fig. 2 shows a typical core analysis obtained by coring with water-base mud. The reservoir has no appreciable dip and is closed on the sides by degradation of sand into shale. The main body of sand is heavily laminated with shale stringers, which are not continuous between wells. The main reservoir is overlain by 30 to 40 ft of laminated low-permeability sand and shale streaks. No information is available on the original properties of

By P. T. Chiang

Chemical etching methods for the simultaneous revealing of the tellurium or selenium Phase and the chalcogenide grain boundaries of the alloy systems are given. A tellurium eutectic was found Present in zone-melted ingots. Similarly, a selenium monotectic was present in ingots. In general, the second phase (tellurium or seleniumn) occubies three different sites; viz., along the chalcogenide grain boundaries, as inclusions within the chalcogenide grain, and on the undersurface of the ingot. The detection limit for the tellurium phase is about 1 u in width. THERMOELECTRIC materials based on Group V (bismuth, antimony) and Group VI (selenium, tellurium) elements have aroused considerable interest in recent years in the practical application of thermoelectric cooling. In many cases, a small amount of excess tellurium (or selenium) was added to the material to optimize its thermoelectric properties. Then the question immediately arises as to the number of phases present in the resultant alloy. In the binary systems of Bi-Te, Sb-Te, and Bi-Se, the congruent melting compositions have been reported to be non-stoichiometric and are represented by Bi~Te respectively. It is to beexpected and known that Bi2Te3 and SbzTe3 crystallize from the melt with an excess of bismuth and antimony in the lattice and that tellurium forms a eutectic.~' The same could be assumed to take place in the pseudo binary systems of (Bi,Sb)zTe3 and Bi2(Se,Te)3 as well as in the system studiedby puotinen5 and other workers. Likewise, BiaSe3 crystallizes from the melt with an excess of bismuth in the lattice and selenium forms a monotectic.~ Therefore, in practice, alloys solidified from the melt often contain a second phase (tellurium or selenium) in one region or another of the solid mass even without the addition of excess tellurium (or selenium). ~u~~recht' studied the thermoelectric properties of (Bi,Sb)2Te3 alloys with excess tellurium and simultaneous additions of selenium. He mentioned that the materials show two phases because of the considerable excess of tellurium or selenium. However, he did not report as to how the tellurium or selenium phase was identified. It is generally believed that the presence of an excessive amount of tellurium or selenium phase in the alloy would adversely affect its thermoelectric properties and its uniformity. Consequently, there is a need for a simple method for the identification of the tellurium and selenium phase. The quantity of the second phase present is usually too small to be detected either by chemical analysis or by normal X-ray techniques. This investigation was therefore carried out, first, to devise a simple metallographic method for the identification of the tellurium or selenium phase coexisting with the chalcogenides and, second, to determine the distribution and specific location of the tellurium or selenium phase in the ingots. EXPERIMENTAL PROCEDURE The starting materials used for the alloy preparations were 99.999 pct pure bismuth, antimony, and tellurium and 99.997 pct pure selenium. The bismuth and antimony were obtained from Consolidated Mining and Smelting Co. of Canada Ltd., while the selenium and tellurium were obtained from Canadian Copper Refiners Ltd. The tellurium was purified further in the laboratory by zone refining. The elements were pulverized in a stainless-steel pestle and mortar. The amounts for the desired composition were weighed out each time on an analytical balance to make up a 100-g sample. Then the sample was introduced into a Vycor ampule (19 by 150 mm), pumped down to a vacuum of 10"5 Torr for 15 min, and sealed off. The ampule was then heated in a horizontal resistance furnace at 800" to 900°C for about 20 hr. During this period the assembly was rocked back and forth several times to ensure good mixing. At the end of the heating period, the ampule was quenched in cold water and then transferred to the zone-melting apparatus described in a previous publications to grow large-size aligned polycrystals. The background and ring-heater temperatures were adjusted to make the freezing solid-liquid interface slightly convex to the liquid. The recorded temperature gradient in the vicinity of the freezing solid-liquid interface was around 15°C per cm. The ampule was moved horizontally at a speed varying from 0.4 to 2 cm per hr so that the ring heater would cover the whole ingot length from end to end. A single zone-melting pass was used for the Bi-Te, Sb-Te, and Bi-Sb-Te ingots. Two passes in the forward and reverse directions were carried out for the Bi-Se and Bi-Se-Te ingots. Six passes in the forward and reverse directions were performed for the Bi-Sb-Se-Te ingot. The zone-melted ingots were found to contain several large crystals, with their basal planes (0001) approximately parallel to the growth axis. Samples of bismuth and antimony tellurides coated with a layer of tellurium, and bismuth selenide coated with a layer of selenium, were prepared for comparison in phase identification. These coatings were made by dropping a piece of the zone-melted ingot into some molten tellurium or selenium under argon atmosphere and allowing them to cool slowly to room temperature. The metallographic specimens were prepared by

Jan 1, 1969

By W. Rostoker

INTRODUCTION THE process of diffusion alloying of mixed powders offers attractive possibilities both commercially and experimentally. It avoids the fabrication difficulties arising from high alloy contents. Indeed, the process is facilitated by larger alloy additions. The direct formation of the part or test piece and the opportunity to perform machining operations under more favorable conditions are of no small importance. However, it is necessary to make only brief mention of the interesting features. As yet there have been few attempts to study this process in detail and to carry it to completion, if such is possible. It was intended not only to measure the intermediate and optimum magnetic properties of sintered alloys but to use magnetic testing itself as a means of following the progress of alloying under various conditions. Having established that alloys could be successfully synthesized by this technique, the opportunity was taken to study the magnetic properties of several alloys of iron and silicon which had hitherto been too difficult to prepare in suitable test piece form, While avoiding some of the difficulties inherent in the fabrication of alloys by orthodox methods, the diffusion alloying process introduces a few of its own. The first of these is the evaluation of the approach to homogenization. In recent years some notable contributions have been made to this question, but considerable uncertainty remains in its definition and evaluation. This work has concerned itself with further study of this problem and it is hoped that more light has been shed on it, The second of these difficulties arises from the presence of porosity. It is inevitable that in the consolidation of a loose bulk of powder, there should remain some voids unless extremely high pressures are repeatedly applied. It was therefore of importance to investigate their effect on magnetic properties. Recently this effect has been studied and certain predictions made of its behavior. It is believed that the experimental results presented here provide a sound substantiation of the theoretical treatment. The attempt has been made to synthesize five alloys of the iron-silicon system and three each of the iron-nickel and iron-cobalt systems. A series of experiments was also conducted on some of these alloys to test their susceptibility to heat treatment. Some unfortunate experiences have provided opportunity to report data on the deleterious effects of nitrogen on magnetic properties when present as a contaminant in protective atmospheres. MATERIALS, PREPARATION OF SAMPLES AND TESTING The purest materials available were employed for this work. A specially purified,

Jan 1, 1948

By George W. Powel

IN the nation's effort to raise its magnesium metal supply to meet the ever increasing demand, the Government is relying not only on standard established practice but has extended its support to developments not so well proved-at least, not commercially proved. Within the past few months considerable progress has been made, not only in the definite output of metal but in the exploitation of new processes, the successful adaptation of which should, in a reasonably short time, assure an adequate supply of magnesium. Recent months have also witnessed a reshuffling of the favored methods as well as of the likely raw materials, with the mineral dolomite gaining in interest over its richer but less abundant competitor, magnesite, while the lowly sea water appears to be losing ground to the higher magnesian brines of Michigan and western Texas. Every month sees a new alignment and there are signs that still newer methods or raw materials will be in use before the industry finally stabilizes itself.

Jan 1, 1942

It has been established that molybdenum sesquisulphide, not molybdenite, is in equilibrium with molybdenum metal and sulphur vapor in the vicinity of 1100°C. The S2 pressure for this system has been obtained using the Knudsen orifice method and the standard free energy for the dissociation of S2. THIS work was undertaken to help in determining the thermodynamic properties of the molybdenum sulphide which is in equilibrium with metallic molybdenum and sulphur vapor in the temperature range 1025" to 1150°C. From the results of MontoroL and of Parravano and Malquori' molybdenite would be expected to be in equilibrium with molybdenum metal, while the results of Guichard indicate that a lower sulphide must be in equilibrium with the metal. Thus it was concluded that the problem warranted reconsideration, especially in view of the suspiciously low temperature independent term for the standard free-energy function for the reaction MoS² Mo + S,. The reaction was calculated and duly noted as being low by Richardson and Jeffes,' using the data of Parravano and Malquori.' Experimental Method The general method used in this investigation is that of the Knudsen orifice method for the determination of equilibrium pressure. The apparatus and technique are similar to those described for the determination of the vapor pressure of silver.% owever, a closed-end McDanel tube instead of fused silica was used to maintain the vacuum, a molybdenum effusion cell with a replaceable lid was employed instead of a silica cell, and a titanium getter maintained at run temperature was used to assure that no oxidation of the molybdenum or molybdenum sulphide was taking place. All runs were made at a residual pressure less than 10-5 mm Hg. The data are given in Table I. Runs 1 through 13 were obtained using molybdenite, analyzed 98.5 pct, from the Molybdenum Corp. of America. The remaining runs were done with a sample from the Climax Molybdenum Corp. which was their grade No. 3 and analyzed 59.87 pct Mo. The weight loss of the cell during heating up and cooling down was subtracted from the total weight loss of the cell during the run. Also, when the tem- perature was changed, the Knudsen cell was placed in the vacuum chamber and heated at temperature for several hours in order to allow the sulphide and the metal to adjust their compositions to the equilibrium values, to desorb or adsorb gases into or from the molybdenum cell itself, and to desorb any water from the molybdenum sulphide or molybdenum powder inside the cell. Water may have been adsorbed inside the cell because, after each run, the top of the cell was removed and the material in the cell was stirred to insure that a layer of molybdenum metal would not build up and obstruct the passage of sulphur vapor into the gas phase. It was established that the molybdenum cell alone decreased in weight an inappreciable amount when heated at the highest run temperature for long periods of time. There are two questions to be answered before the data in Table I can be used to calculate thermodynamic functions: 1—Which molybdenum sulphide is in equilibrium with molybdenum metal and sulphur vapor? 2—What sulphur species are present in the vapor phase? It can be assumed safely that no molybdenum is vaporized, since its vapor pressure is almost negligible at these temperatures. It will be shown subsequently that no sulphide of molybdenum is volatile. Question 1 was answered in the following way: The especially purified molybdenite, obtained from the suppliers mentioned previously, was charged

Jan 1, 1956