Search Documents

INTERNATIONAL ENGINEERING CONGRESS This Congress will be held under the auspices of five National Engineering Societies, of whi h the Institute is one. The sessions will be held in 11 sections and the proceedings will be published in 10 volumes of 500 pages each, of which Volume 8 will contain the papers and proceedings on Mining Engineering and Metallurgy. The membership fee of $5 will entitle the holder to the volume of General Proceedings and Index, and, in addition thereto, any other single volume chosen. Other volumes may be subscribed for according to a sliding scale depending upon the number of volumes taken. The Institute will have a meeting in San Francisco during 1915, and it is desirable for our members to join the International Engineering Congress at in early date in order that their support of the enterprise may be given in its early stages, when it is most needed.

Jan 2, 1914

By James E. Harding

AT just about the geographical center of the peninsula of Lower California is the El Arco gold mine. It is small and spotty, and three separate attempts to operate it in the past have failed. The only reason the present operation is possible is because of the higher price of gold and because the previous operators had spent about $300,000 developing the property with shafts, four levels, machinery, and a complete mill, all of which was acquired at a bargain price. All the known ore in the mine, to say nothing of the cost of recovering it, is

Jan 1, 1937

E. G. WOODRUFF, Houston, Tex. (communication to the Secretary*). -Mr. Matteson has presented to us an idea worthy of our careful consideration. We have real troubles in the petroleum industry and as the supply of crude is exhausted our problems become more complicated and more numerous. Therefore, we who are engaged in field work are forced to consider all possible means which promise assistance in the location of prospective pools and the economic development of pools already located. In our country we are accustomed to turn to the. Government for relief in all our troubles. Do we want an Oil and Gas Bureau doctoring us? Will such a bureau do us practical good? The principal point Mr. Matteson suggests is that such a bureau should he authorized to receive and file all well logs. In analyzing such function, I am led to the following conclusions: If well logs are simply to be filed they would be useless. If they are to be filed and the files opened to the public, what benefit will be derived and can such action be taken justly? There is no doubt that if the record of all wells drilled in the United States were available the petroleum industry would be saved an immense amount of needless expense. Accumulating conditions would be better understood and prospecting more intelligently directed. Our other consideration is: can the oil companies be required to open well records to the public justly? I think all will agree that if any one should have the advantage of a well record it should be the company that drilled the well. If the oil companies are forced to file such record and open the files to the public, the company drilling the well cannot derive the exclusive benefit from the money expended. Would it be just for a small company to be compelled to reveal its records of a well it had recently completed, to its strong competitor who holds near or even adjacent leases? Would it have been just to the successful companies, in the Gulf Coast country to have been forced to display their hard-earned knowledge of 15 years to the host of younger competitors who have recently flocked to the Gulf Coast attracted by the success of those who have labored so long and learned of the conditions controlling the fields through the hazards of the industry.

Jan 10, 1917

By E. S. Leaver

THE presence of soluble base metals in precious-metal ores usually precludes cyanidation as the best method of treatment. The laboratory experiments described in this paper show the possibility of cyanidation of gold-silver ores containing less than 0.5 per cent. of cyanide-soluble copper and the effect of zinc in the cyanide solution. PART 1.-COPPER IN CYANIDATION The proposed process of cyanidation of precious-metal ores containing copper is based on the regeneration of about 80 per cent. of the cyanide used in the dissolution of the copper. The method of regeneration involves a combination of the sulfide and the acid precipitation of the copper and silver. The resultant solution is made alkaline with lime, and the gold is precipitated with zinc dust.

Jan 1, 1929

By Harmel A. Dawson, Robert A. Wilson

First the basic steps to determine the values present and the minerals involved which are the basis for the metallurgical testing are presented in this paper. Next, choosing the process or processes indicated for treating an ore are discussed. This is followed by the test procedures used, the results of which will indicate amenability to treatment. These test procedures have been developed, used and proven effective in laboratory evaluations relative to plant processing. Special, uncommon processing is beyond the scope of the paper. Evalutation of test results and incorporation into the preliminary and final flow sheet for plant design are discussed. The value of a flow sheet, with material and water balances, to plant design is shown.

Jan 1, 1978

By P. Somasundaran, D. W. Fuerstenau

The length of the collector is found to influence the flotation of the mineral even at incipient conditions, which are below the concentration at which interaction at the solid-liquid interface begins to take place to form hemi-micelles. To study this dependence, concentration for incipient flotation of quartz was determined as a function of pH with collectors of various chain lengths. The observed effect of chain length on flotation is ascribed to that of collector adsorbed on the bubble surface. In previous studies, it was shown that at low concentrations the alkyl collector ions adsorb at the solid-liquid interface as individuals.''2 At higher concentrations, the collector ions adsorbed at the solid-liquid interface associate with each other to form two-dimensional aggregates called hemi-micelles. Above the hemi-micelle concentration, the length of the hydrocarbon chain is extremely important since the hydrocarbons are in effect removed from water during the association, making the energetic conditions more favorable for adsorption at the interface. Because of this enhanced adsorption, one observes a very rapid increase in flotation associated with the hemi-micelle formation at the solid-liquid interface. However, a dependence of flotation on the chain length at concentrations below that required for hemi-micelle association was also observed,' and this cannot be explained by the above mechanism which postulated hydrocarbon chain interactions only at the solid-liquid interface. This prompted an investigation into other possible reactions of the hydrocarbon chains and an examination of the conditions at the bubble surface involved in the flotation system and how these observations might explain the reactions at the solid-gas interface which cause the particle-bubble attachment required for flotation. To obtain more information on chain length effects, flotation, under incipient conditions, was tested by vacuum flotation techniques. The collector-concen-tration-pH relationships for flotation of quartz with alkyl ammonium acetate collectors was delineated by observing the pH at which quartz particles begin to float to the liquid surface. By investigating flotation as a function of pH, it was also possible to study the effect of neutral molecules on incipient flotation conditions, since the aminium ions hydrolyze to amine molecules at higher pH values. EXPERIMENTAL WORK Brazilian quartz specimens were crushed and sized, and the 270 x 400 mesh fraction was used for flotation studies. The samples were leached with concentrated hydrochloric acid until no coloration of the acid occurred. The leached material was washed free of chloride ions and stored in distilled water. The vacuum flotation technique developed by Schuhmann and prakash3 was used to determine the critical pH-concentration curves. This method, which can be used to delineate conditions for incipient flotation, is fairly simple and rapid. About 0.5 gm of 270 x 400 mesh quartz was placed in a 100 ml graduated cylinder which was then filled to the 100 ml mark with the collector solution made from high-purity alkyl ammonium acetate salts. The water used for the test was conductivity water saturated with air that had been passed through a cleansing train consisting of Drierite, Ascarite, a water wash bottle, and a trap. After the pH was adjusted, the cylinder was then conditioned for thirty minutes. In the tests where an acid pH was desired, sufficient acid was added before the collector solution to avoid any effect due to slow desorption of collector from the quartz surface. After conditioning, vacuum was applied to the system and the flotation or nonflotation of the quartz was noted. The pH at which the quartz particles began to float to the liquid-gas interface was taken as the critical PH. Critical pH curves were thus determined for different concentrations of the various collectors. Hallimond tube flotation data were taken from the authors' previous publication1 for correlation with that from the vacuum flotation. RESULTS AND DISCUSSION The results of vacuum flotation studies for determining critical pH-concentration curves, i.e., curves which delineate conditions for incipient flotation, are shown in Fig. I. In generaI, all the curves exhibit an upper and lower pH limit between which flotation will

Jan 1, 1969

All the TECHNICAL PUBLICATIONS and CONTRIBUTIONS published in 1935 are available at Institute headquarters, unless otherwise noted. They are also on file in many public, university and technical libraries and, when so indicated in the list, may be found in the TRANSACTIONS. Copies of the TECHNICAL PUBLICATIONS have been mailed to members of the Institute that are registered in the different classes: A-Metal Mining; B-Milling and Concentration; C-Iron and Steel Division; D-Nonferrous Metallurgy; E-Institute of Metals Division; F-Coal Division; G-Petroleum Division; H-Industrial Minerals Division (Nonmetallics); I-Mining Geology; J-Mineral Industry Education Division; K-Mining Administration; I-Geophysical Prospecting. Other members may obtain copies by writing to the Secretary. Copies of CONTRIBUTIONS may also be obtained from the Secretary's office. Additional copies are sold at the rate of 1 cent per page; minimum charge, 25 cents. Nonmembers may purchase the papers at the prices mentioned. [ ]

Jan 1, 1936

By Neil Donnell, O&apos

MODERN mine maps are largely a product of evolution. The first mine maps used in the west were old composite maps with all the levels plotted on the same sheet. The composite was widely used and occasionally is seen even now. This type of underground map had serious limitations. One was the development of an indecipherable complex of workings around steep shafts. The other limitation was that of size; often when a working passed the limit of the sheet no map was made of it. These old maps have been superseded by the single level maps, laid out in squares or rectangles which can be expanded indefinitely in all directions. This produces a system capable of unlimited expansion in three dimensions, with all the detail of every working clearly marked and legible. A good set of mine maps should be laid out in blocks, all blocks of equal size. Each block should be limited by plane coordinates without overlap on bounding map quadrangles. At all times the direction of North should be indicated as an aid in remembering bearings of underground workings. It is desirable that all maps of whatever scale be plotted on sheets of uniform size. In fact, it is possible to make nearly all underground maps, surface maps and sections on sheets of the same size.

Jan 9, 1950

By Joseph L. Gillson

BRAZIL has had an industry based on ocean beach deposits of heavy minerals containing monazite, zircon, rutile, and ilmenite for well over 40 years, but except at the very earliest period, prior to 1906, and again during World War 11, has this industry been at all comparable in size with similar operations in other countries. Limiting factors have been neither a lack of reserves nor lack of markets (except for zircon). Although poor local transportation and shipping facilities have handicapped the development in Brazil, these conditions were perhaps equally bad (when mining operations started) in the Indian State of Travancore, and in New South Wales and Queensland, Australia, in which states the principal production of beach deposits of heavy minerals has occurred. The outstanding restraints on the Brazilian industry have been the lower quality of the Brazilian minerals, the relative small size of individual deposits that were known until recently, the lack of interest of Brazilian investors in mining ventures, and the unfavorable climate for investment of foreign capital under Brazilian mining law. The lower quality of the minerals is indicated by the fact that the Brazilian monazite carries only 5 to 6 pct ThO2,*, and the ilmenite 56 1/2 pct TiO2, whiteness of the Australian zircon. An inadequate market for the abundant zircon that will be avail- able in any operation in Brazil is certainly a heavy restraint, since otherwise it could be an important byproduct. The oxide of zirconia, baddeleyite, that has come from Brazil is from other sources. 1 Since the Brazilian beach sands carry only a little rutile, that mineral has not been available as a valuable byproduct to help finance the operations.

Jan 6, 1950

By R. W. Kobler, D. A. Dahlstrom

Since the development of the pelletizing process in the fifties for relatively high purity pellets from low grade taconites, there have been several distinctive changes in filter construction for the dewatering step preceding balling. In the original large pilot plant run by Reserve Mining Co. in Babbitt, MN, the disk type filter employing agitation (Agidisc filter) was selected as the most economical. Size was limited to 2.1 m (6 ft, 9 in.) in diameter. The second generation occurred in the sixties with a jump to 2.70 m (8 ft, 10 in.) in diameter to reduce capital costs per annual ton of pellet. In the early seventies, the third generation was the steam drying disk filter which became necessary to achieve balling moistures with specific surface areas of 2200 cm2/g to as high as 3800 cm2/g caused by finer grinding to obtain higher purities. Finally, the fourth generation has recently been developed to reduce maintenance costs and further improve hydraulics to ensure minimum moisture contents.

Jan 1, 1980

By C. V. Millikan, Herbert F. Beardmore

Declining Productivity Index, as considered herein, is a productivity index that has a substantially and consistently decreasing value when measured over a period of a few hours. If not recognized, it may be interpreted as representing an unsettled or unstable condition in a producing well. It forms the basis of a number of predictions as to future performance compared with the performance of wells in which the productivity index does not decline. The nost important of these are that: (I) the rate of oil production will decline more rapidly, (2) the gas-oil ratio will usually increase abnormally, (3) the amount of water ultimately produced will be negligible, if any, (4) stop-cocking will increase current production and decrease gas-oil ratio. When such relative well performance is indicated, it follows that certain reservoir performance and operating practices may be anticipated: (I) disappointing recovery, (2) longer natural flow, (3) no active water drive, (4) better evaluation of acidizing, shooting and reworking, (5) intermittent operation of wells, (6) smaller pumping equipment required. It is significant that the basis of these important predictions is bottom-hole pressure tests that can be made immediately after completion of the wells. Introduction "'Productivity index" is the number of barrels of oil produced per day per pound per square inch of differential pressure between the reservoir and the bottom of the well. "Declining Productivity Index," as considered herein, is a productivity index that has a substantially and consistently decreasing value when measured over a period of a few hours. Productivity index can be determined only when the rate of production can be stabilized. In most wells the rate of production and bottom-hole pressure are easily stabilized to give a constant productivity index for a period of many hours. A few produce so erratically as to preclude probability of an acceptable test in the usual sense. A satisfactory productivity index can be determined in some wells only by gauging the production accurately by hours, measuring the bottom-hole pressure continuously, and from these data calculating the productivity index for successive hours. Such figures frequently will have a decreasing value—that is, a declining productivity index—and when plotted on double. logarithmic cross-section paper with productivity index as ordinate and time as abscissa will be a straight-line curve. The angle between the curve and the abscissa is referred to as the rate of decline. Declining productivity index may appear to be the result of change in permeability to oil due to decreasing saturation of oil and increasing saturation of gas in the reservoir. It is possible that such is in fact the cause, but if so, more is involved than merely relative saturation of oil and gas. This seems evident because the rate of decline in productivity index is substantially the same regardless of the pro-

Jan 1, 1945

By E. S. Machlin, C. W. Chen

THIS investigation is concerned with the origin of the intercrystalline voids and cracks formed in metals and alloys subjected to stress at elevated temperature. There have been many suggestions in the recent literature relating to this problem. Greenwood' suggested that the voids may be produced by vacancy condensation. Zener has stated that shear-stress relaxation across grain boundaries could initiate high tensile stresses at the regions blocking grain boundary slip and thereby cause the formation of cracks. Chang and Grant3 have described the formation of cracks at grain boundary triple points and have experimentally verified Zener's mechanism for the grain boundary regions in the vicinity of a triple point. Subsequent to the completion of this investigation, Gifkins4 developed a model which made use of Stroh's5 mechanism of fracturing to produce sub-microscopic fractures that subsequently grow by grain boundary slip. Chen and Machlin,6 in answer to Gifkins, described a model deduced from the present investigation, in which grain boundary slip provides both the stress to fracture at grain boundary jogs and the deformation required to separate fractured jog surfaces. The possibility of gas condensation to form intercrystalline voids and cracks is eliminated as a basic mechanism because such voids and cracks are developed in vacuum melted material containing minute amounts, if any, of gaseous impurities. In a theoretical evaluation of this problem, Machlin7 concluded that void nucleation by vacancy condensation during creep-rupture is improbable but that vacancy condensation on supercritical sized voids to produce growth is probable. This investigation was begun to evaluate the suggested mechanisms for intercrystalline fracture. In particular, in order to correlate vacancy supersaturation ratios produced in creep with those determined by Bal-luffi and Seigle8 as critical for , the nucleation of voids, specimens were obtained from the same heat of brass as used by the latter authors, through the courtesy of Dr. Seigle. The experiments conducted in this investigation fall into the following categories: 1) Brass—observation of voids produced under a variety of conditions, including creep under compression, to evaluate the mechanisms of void nucleation and growth. 2) Bicrystal experiments to check the mechanism of void nucleation deduced in this investigation. 3) Morphology of intercrystalline voids produced in a variety of metals. Each set of experiments will be described and discussed separately. Experimental Techniques A special creep-rupture test rack was constructed which made it possible to apply the stress to the specimen in a controlled atmosphere of inert gas, reducing gas, or vacuum. All the creep-rupture tests on a-brass (30 pct Zn) were conducted in nitrogen under a pressure slightly above atmospheric. Either dead weight loading or constant elongation rate loading could be applied with the load measured by means of a strain gage dynamometer. In order to obtain a coarse-grained crystal structure stable at

Jan 1, 1958

By A. F. Bertuzzi, M. R. Tek, F. H. Poettmann

A method is presented for predicting pressure drop for two-phase fluid flow in horizontal pipes. A set of 267 experimental measurements randomly sampled from approximately 1,000 measurements from various literature sources was used. Pressure gradients calculated by the procedure developed and compared with the experimental values showed a bias of +0.82 per cent and a standard deviation of 20.8 per cent. The advantatges of this method over other available methods of predicting two-phase flow pressure drop are (a) its comparative simplicity of application, (b) its relative independence of flow patterns, (c) its accuracy, which on the basis of a statistical evaluation predicts pressure drop closer than other available methods, and, (d) its ability to satisfactorily correlate laboratory data from various sources while the correlations from these sources do not appear to agree with one another. The method has been reduced to a simplified graphical procedure, suitable for field use. A two-phase f factor is defined and correlated with parameters involving the flowing gas-liquid mass ratio, a Reynolds number for the gas phase, and a Reynolds number for the liquid phase. The choice of parameters allows the correlation to reduce to the usual f factor plot for the limiting conditions of (111 gas or all liquid. INTRODUCTION The mechanics and characteristics of two-phase flow systems have been of interest throughout the industry for some time. In numerous engineering installations such as pipe lines, chemical reactors, and heat exchangers, two-phase flow conditions are of every day occurrence. In oil production operations it has been desirable, in some cases, to consider transporting gas and oil together in a common pipe from oil field to process plant. The trend toward centrally located stock tank batteries in oil fields has resulted in longer gathering pipelines in which more than one fluid phase is flowing. The increase in the producing capacity of oil wells due to new production tech- niques has created the need for review and re-design of many surface gathering lines for properly handling the increased production. Optimum pipe size for the situations described above has become an important factor. The problem which is of interest here involves the ability to predict the relationship between pressure drop, fluid properties, fluid rates, pipe diameter, and pipe length. Although the literature1,5,10,13,18,19 contains various articles dealing with specific cases of the problem, Lock-hart and Martinelli17 proposed the most general solution. Their method has been later modified by Baker:1 Alves2 demonstrated that different flow patterns are possible for a flow mechanism defined by Martinelli such as gas turbulent, liquid turbulent. Baker explained deviations experienced with Martinelli's correlations on the basis that different flow patterns could exist for the same flow mechanism. Using Martinelli's method of correlatioil, Baker correlated data for each flow pattern for the turbulent-turbulent flow mechanism. Bergelin and Gazley6,7 presented a correlation for predicting gas phase

Jan 1, 1957

By Thomas S. West

A gravel pack completion is described which, in addition to sand screening, permits the exclusion of water and gas from the oil production. A gravel pack composed of alternate layers of different particle sizes is employed which has horizontal but not overall vertical permeability to drilling mud. A packer is run on the tubing and set in the screen member, around which the gravel layers are placed. The hydrostatic pressure of a mud column prevents the entry of fluid above (or below) the level of the packer. The producing level may be changed by raising or lowering the tubing. Vertical coning is controlled by replacing the mud column with oil and continually injecting oil into the sand section above (or below) the packer. Three well histories with this completion are described in detail. Statistics on the first 100 completions of this general type are given. INTRODUCTION Gravel pack type completions have heretofore been almost exclusively for the purpose of preventing sand production. This paper describes and presents well data on a gravel pack procedure which is primarily a selective completion method. Although complete sand screening is achieved, the exclusion of gas and water is the primary objective. The application of this procedure is therefore not limited to unconsolidated sands. Application to hard sand or limestone reservoirs is equally feasible. GRAVEL PACK PROCEDURE Figs. 1 and 2 illustrate the gravel pack procedure employed. The gravel is placed by means of the frangible disc type dump bailer shown by Fig. 1.' This bailer has its lower end closed by a plate glass or steel rimmed cement disc. This disc breaks when the bailer passes over the liner allowing the gravel to be deposited around the liner. The liner employed is usually 2 3/8 in. to 2 7/8 in. OD and 1.995 in. or 2.07 in. ID (ID of 2-in. tubing or 2-in. line pipe). Two tvDes,. of slotted sections have been employed. One type employs horizontal hacksaw cut or milled slots of about 1/32 in. width opposite the producing section. The other type employs the same type,. of horizontal slot. but slots are placed in groups of six at intervals of about 8 in. A cage composed of half round vertical bars, spaced apart, is then welded to the pipe over the slotted sections. This liner has the bottom end closed, usually by bull plugging. The upper end is closed, while placing the gravel, by a cap which is held in place by means of a shear pin. This cap has a mandrel attached to it which extends downward inside of the liner to within a few inches of its lower end. The top of the liner cap is formed to fit a releasing type wire line core barrel overshot. The liner is lowered to bottom on the wire line by means of this overshot and released. The length of the liner is usually suffi- cient to extend to about 20 ft above the highest level to which gravel is to be placed, the upper end of the liner always being in the casing. The dimensions of the liner and bailer are such with respect to the casing size that the bailer will always pass over the liner. After releasing the liner the bailer is run to bottom. Passage of the empty

Jan 1, 1951

By Thomas S. West

A gravel pack completion is described which, in addition to sand screening, permits the exclusion of water and gas from the oil production. A gravel pack composed of alternate layers of different particle sizes is employed which has horizontal but not overall vertical permeability to drilling mud. A packer is run on the tubing and set in the screen member, around which the gravel layers are placed. The hydrostatic pressure of a mud column prevents the entry of fluid above (or below) the level of the packer. The producing level may be changed by raising or lowering the tubing. Vertical coning is controlled by replacing the mud column with oil and continually injecting oil into the sand section above (or below) the packer. Three well histories with this completion are described in detail. Statistics on the first 100 completions of this general type are given. INTRODUCTION Gravel pack type completions have heretofore been almost exclusively for the purpose of preventing sand production. This paper describes and presents well data on a gravel pack procedure which is primarily a selective completion method. Although complete sand screening is achieved, the exclusion of gas and water is the primary objective. The application of this procedure is therefore not limited to unconsolidated sands. Application to hard sand or limestone reservoirs is equally feasible. GRAVEL PACK PROCEDURE Figs. 1 and 2 illustrate the gravel pack procedure employed. The gravel is placed by means of the frangible disc type dump bailer shown by Fig. 1.' This bailer has its lower end closed by a plate glass or steel rimmed cement disc. This disc breaks when the bailer passes over the liner allowing the gravel to be deposited around the liner. The liner employed is usually 2 3/8 in. to 2 7/8 in. OD and 1.995 in. or 2.07 in. ID (ID of 2-in. tubing or 2-in. line pipe). Two tvDes,. of slotted sections have been employed. One type employs horizontal hacksaw cut or milled slots of about 1/32 in. width opposite the producing section. The other type employs the same type,. of horizontal slot. but slots are placed in groups of six at intervals of about 8 in. A cage composed of half round vertical bars, spaced apart, is then welded to the pipe over the slotted sections. This liner has the bottom end closed, usually by bull plugging. The upper end is closed, while placing the gravel, by a cap which is held in place by means of a shear pin. This cap has a mandrel attached to it which extends downward inside of the liner to within a few inches of its lower end. The top of the liner cap is formed to fit a releasing type wire line core barrel overshot. The liner is lowered to bottom on the wire line by means of this overshot and released. The length of the liner is usually suffi- cient to extend to about 20 ft above the highest level to which gravel is to be placed, the upper end of the liner always being in the casing. The dimensions of the liner and bailer are such with respect to the casing size that the bailer will always pass over the liner. After releasing the liner the bailer is run to bottom. Passage of the empty

Jan 1, 1951

By G. Das, S. V. Radcliffe

The substructural features developed in tungsten as a function of annealing temperature (up to 2200°C) and type of material [undoped and doped powder metallurgy (PM) tungsten and electron beam melted tungsten] have been investigated by transmission electron microscopy. For doped PM tungsten wires, characteristic "par-ticulate" substructural features developed rapidly with increase in annealing temperature above 700°C. The features consisted of parallel rows of elongated or circular shapes (500 to 1000A diam) lying along the direction of the wire axis and were identified as internal voids by diffraction contrast experiments. In recrystallized doped PM rod, larger voids were observed and were identified by precision dark field analysis to be cubic in shape and bounded by (100) planes. In marked contrast with both the doped PM materials, recrystallized undoped PM rod exhibited only very occasional and randomly arranged voids. Furthermore, no voids were observed in either material after electron beam melting. The high concentration of voids in the doped PM materials is attributed primarily to vaporization of doping additions or their pvoducts situated at the original grain boundaries , whereas the few voids in undoped material are considered to be traces of microporosity which were not eliminated during sintering. A tentative mechanism is suggested for the dezlelopment of the voids in relation to the processing sequences (sintering and working) and to the subsequent annealing. In recent years, a characteristic substructural feature consisting of rows of small elongated or circular regions of light contrast lying along the direction of working has been seen in thin foil electron microscopy studies of annealed sheet, wire, and rod tungsten. These features were present in the published micrographs of sheet by Weissmann et al.1 and of wire by Meieran and Thomas2, although the authors did not draw attention to them. Wronski and Fourdeux3 observed similar features in sintered rod tungsten (it was not specified whether or not the material was doped*) and interpreted them on the basis of their ap- particles, based on extraction replica evidence from the fracture surface of the initial hot-rolled slab material from which the sheet was prepared. No diffraction contrast experiments on the features were reported in any of these studies. The present investigation was undertaken with the primary objectives of: a) identifying the nature of these substructural features in tungsten by electron diffraction contrast experiments, since the contrast for voids can be expected to differ from that for crystalline or glassy particles, and b) elucidating the origin of the features and their development. For the latter purpose, doped and undoped powder metallurgy tungsten was obtained as rod and wire to represent different stages of reduction during final processing. These materials were examined both in the as-processed condition and after annealing to successively higher temperatures. In addition, the same doped and undoped materials were examined after vacuum melting in rod form. I) MATERIALS AND PROCEDURE Doped powder metallurgy (PM) tungsten wire (commercial purity 99.9 pct W) was obtained in the as-drawn and surface ground condition (0.030 in. diam "ground seal rod"). Doped and undoped tungsten rod (0.075 in. diam) representing an earlier stage of final processing was obtained from the same commercial source (Refractory Metals Division, General Electric Co.). Lengths of both the doped and undoped rod materials were single-pass melted in an electron-beam zone refiner to examine the effect of vacuum melting on the substructure. Annealing was carried out in a tungsten crucible in a tantalum strip resistance furnace under a vacuum of l0-15 mm Hg. Longitudinal sections of the wire and rod materials were examined by light and electron microscopy. The preparation of thin foils suitable for electron transmission from 0.030 in. diam tungsten wire and the rod specimens was carried out by means of a high-precision microjet technique developed to provide lack of jet stability and precise control of the area thinned. The method is described in detail elsewhere.' The foils were examined in a JEM 6A electron microscope using a goniometer stage (±20 deg tilt, 360 deg rotation) and operated at 100 kV. To minimize contamination problems a 200 µ condenser aperture was used in conjunction with a useful beam current of 50 µA. II) RESULTS AND DISCUSSION A) Diffraction Contrast Analysis. In order to determine the optimum conditions for the development of the substructural feature, a series of isochronal 30 min annealing experiments were carried out on specimens of the doped PM tungsten wire. The transmission electron microscopy analysis showed that the as-drawn wire, Fig. 1(a), consists of 'fibers' whose long axis is closely parallel to the wire axis of (110). The fiber width averages some 0.5 µ. Dense disloca-

Jan 1, 1969

By Niels Hansen

Dispersion-strengthened sintered aluminum products are normally manufactured from surface-oxidized aluminum powder, SAP,' or from atomized aluminum powder.' The powder-blending technique consisting in mechanical mixing of the constituents has been used in the manufacture of numerous dispersion-strengthening alloys, but has never been successfully applied to aluminum alloys. This technique may, however, be applicable if it is possible to produce an unagglomerated mixture of the constituents in the form of fine powders, and the present study was initiated to test this assumption in the aluminum/aluminum oxide system.3 Table I lists the two grades of aluminum powder and the aluminum oxide powder used in the manufacture of the alloys. MD 105 A is an aluminum powder with an average grain size less than 5 IJ., which is isolated from the MD 105 powder by centrifugal separation in cyclohexanol. The aluminum powders and the aluminum oxide were blended in a high-speed blender and then subjected to cold compaction and hot compaction at 550" to 600°C. Subsequently the compacts were hot-extruded with an extrusion ratio of 15 to 1. The alloys were evaluated by tensile testing at room temperature and at 400°C, microscopic examination, and heat treatment at 500°C followed by tensile testing at room temperature. For the purpose of comparison, a commercial SAP quality supplied by Swiss Aluminium Ltd. was tested in the same manner. The tensile data at room temperature and at 400°C are plotted in Figs. 1, 2, and 3 as a function of the weight percent of oxide. The oxide content

Jan 1, 1964

By J. Waldman, M. B. Bever, A. K. Jena

The heats of formation at 273°K of 6 silver-rich Ag-Cd solid solutions and the heat of formation at 78°K of one solid solution have been measured by tin solution calorimetry. The heats of formation are analyzed in terms of the quasichemical theory. If the enthalpy diffel-ence between a hypothetical fcc form and the hcp form of cadmium is taken into account, this analysis does not lead to the conclusion put forth in the literature that electronic effects make significant contributions to the heats of formation of silver-rich Ag-Cd solid solutions. The temperature dependence of the heats of formation is appreciable and negative near 78ºK, but decreases gradually to nearly zero abore 400°K. The relative partial enthalpies per grarn -atom of silver at 541°K and cadmium at 532" and 541°K in tin have also been determined. THE composition range of the silver-rich Ag-Cd solid solutions stable at room temperature extends to about 40 at. pct Cd. Heats of formation of these solid solutions at 308" and 723°K have been measured by solution calorimetry.1,2 Heats of formation for an average temperature of 800°K have also been calculated from vapor pressures.2,3 The heats of formation deviate from the values predicted by the quasichemical theory above about 30 at. pct Cd. This deviation has been attributed to electronic effects at the Brillouin zone boundaries.2 The heats of formation of Ag-Cd alloys are essentially the same at 308", 723", and 800°K; consequently the temperature dependence of the heat of formation d?H/dT = ?Cp is vanishingly small, although from the exothermic heats of formation a negative value would have been expected. In the investigation reported here the heats of formation at 273°K of 6 silver-rich Ag-Cd solid solutions and the heat of formation at 78°K of 1 solid solution have been measured by tin solution calorimetry. The results are analyzed in terms of the quasichemical theory and the dependence of the heats of formation on temperature is discussed. The relative partial enthalpies per gram-atom of silver in tin at 541" and cadmium in tin at 532" and 541°K were obtained in the course of this investigation. The values of the temperature dependence of the relative partial enthalpies per gram-atom of silver in tin derived from the data reported by various investigators2,4-9 are contradictory. The literature contains only a value for 517°K of the relative partial enthalpy per gram-atom of solid cadmium in tin.2 EXPERIMENTAL PROCEDURES Samples of Ag-Cd solid solutions were prepared by melting weighed amounts of silver (99.99 pct pure) and cadmium (99.95 pct pure) in graphite crucibles under a flux of molten potassium chloride.10 The solidified ingots were sealed in evacuated Vycor tubes and annealed at 775°K for 10 days. The ingots were swaged and drawn into wires. The wires, sealed in evacuated Pyrex tubes, were held at 725°K for 5 hr and cooled to 365°K at an average rate of 2.5ºK per hr, followed by furnace cooling to room temperature. Chemical analysis of samples taken from different parts of each ingot gave no indication of segregation. Metallographic examination showed the samples to be homogeneous. Samples of the solid solutions or of the component elements were added to tin-rich baths in a calorimeter." At the start of a run the bath consisted of pure tin. Silver was used in the form of wire of 0.01-in. diam as supplied and cadmium in the form of lumps. Gold (99.999 pct pure) was added with the samples in order to reduce the endothermic heat effect of additions of Ag-Cd solid solutions. Samples of only one composition were added in a run and the ratio of the weight of alloy to that of gold was the same in all additions of a given run. In each run several calibrating additions of tin were made from 273°K. The heat contents of tin were calculated from the following equation, which is based on published data:12 (HTºK- H279º) = 6.70 T - 72,300/T + 20 cal/gram-atom; 505°K < T < 650°K The heat effect of each addition was plotted against the average of the sum of the atom fractions of solutes in the solution before and after that addition. The total concentration of solutes at the end of a run was less than 2 at. pct. In this range the heat effect was a linear function of the atom fraction of the solutes. The heat effect at infinite dilution and the composition dependence of the heat effect were obtained from the plots. RESULTS AND DISCUSSION Evaluation of Data. The linear dependence on composition of the heat effects of additions suggests that in the dilute range the enthalpy interaction coefficients other than the first-order coefficients of silver, cadmium, and gold are negligible, as shown in a concurrent publication.13 The heat effects at infinite dilution and the values of the composition dependence of the heat effects are listed in Table I.

Jan 1, 1970

ALABAMA Auburn.-Brown, R. L. Battelle.-Green, G. G. Bessemer.-Abbott, C. E. Dobbs, G. G. Ferguson, V. Birmingham.-Aldrich, T. H. Aldrich, T. H., Jr. Allen, A. W. Bonnyman, J. Bowron, J. Crawford, G. G. Crockard, F. H. Ellis, E. E. Fairbairn, C. T. Gambrill, G. T., Jr. Geismer, H. S. Hiller, E. McCormack, G. B. Maben, J. C.

Jan 1, 1917

By T. G. Richardson, F. M. Perkins

In the recent paper of Richardson and Perkins entitled "A Laboratory Investigation of the Effect of Rate on Recovery of Oil by Water Flooding,"&apos; the authors found very little appzrent effect on oil recovery of having free gas saturation present prior to water flooding in unconsolidated sands. We agree that the effect in this particular system was small but do not feel that the data presented should be regarded as disproving work of others which has shown an appreciable effect. The authors do not make such a claim, but neither do they advance an explanation of the difference. In our experience the following factors must be carefully considered when studying the relation between residual oil saturation after water flooding and initial free gas saturation: (1) the magnitude of the inherent residual oil saturation, i.e., the residual oil saturation with no free gas; (2) the increase in oil-water viscosity ratio with pressure lowering if the gas saturation is obtained by solution gas drive; and (3) the oil shrinkage which occurs with pressure lowering and gas evolution. The system studied by Richardson and Perkins gave residual oil saturations as low as 20 per cent without free gas present, and one should perhaps not expect much further lowering. As an illustration of the magnitude of the effect when the residual oil saturation is inherently higher we submit the accompanying figure. These data were obtained on an unconsolidated sand under elevated pressure in a system similar to the one described by Richardson and Perkins. Gas saturation was established by gas drive before water flooding. The viscosity ratio was 600:1 under the conditions of the displacement. Here the gas was extremely effective in reducing residual oil saturation. This fact was also indicated by Kyte, et al.2 Their plots of residual oil saturation vs initial gas saturation show trends of greater free gas effect with higher oil viscosities. The pressure-dependent effects were not discussed by Richardson and Perkins. They should be separated from the free gas effect if the objective of the study is a correlation of residual oil saturation vs initial free gas saturation. The increase in oil viscosity when gas is released from solution tends to increase residual oil saturation. This effect is rather small in the viscosity range of kerosene. A Buckley-Leverett calculation, assuming an increase in viscosity ratio from 1.2 to 1.8, indicates an increase in residual oil saturation of about 1 per cent of pore volume. Thus, one would expect this system, if operated at constant viscosity ratio, to show a slightly greater free gas effect. As Dyes- as shown, oil shrinkage can offset the beneficial effect of free gas on waterflood oil recovery, if the gas saturation is established by depletion. Since

Jan 1, 1958