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By H. T. Kennedy, S. G. Dardaganian, J. L. Clanton

This paper presents equilibrium ratios measured on oil and gas samples taken from the Kelly-Snyder field at the reservoir temperature of 128°F. From these data smoothed curves were constructed for the reservoir fluid up to the bubble-point, 1,874 psia. A material balance calculation, based on the use of equilibrium ratios instead of the usual solubility and shrinkage meayr~rements is made on the field and compared to the con\.entional method. DETERMINATION OF EQUILIBRIUM RATIOS The equilibrium ratios, or K values were obtained by recombining separator samples of oil and gas taken when the reservoir was above its bubble point, and thus represented the reservoir fluid before any change had occurred due to the evolution of gas. The well sampled had a gas-oil ratio of 617 cu ft of high pressure sepalator gas per barrel of separator oil. and a bottom-hole temperature of 128°F. Samples were brought to equilibrium by agitating for 24 hours in a thermostat, maintained at the proper temperature within 0.2ºF, mercury being added when necessary to maintain the pressure constant. Samples of oil and gas were then taken by constant pressure displacement, and analyzed by low temperature frac-tionation. Equilibrium ratios were determined at 128°F and 500, 800, 1,000 and 1,400 psig. At the latter pressure, there were indications that the gas samples were contaminated with small quantities of oil, and only data taken at the first three pressures were included in Fig. I. This figure has been extended to higher and lower pressures by the use of the Fluor charts for 3,000 psi convergence pressure, on which the experimental points fit well. MATERIAL BALANCE EQUATIONS The possible errors involved in conventional material balance equations have been analyzed by Muskat1. Where the errors occur in field measurements, or in obtaining effective averages from variables such as gas-oil ratio and pressure, they will evidently be involved in any attempt to estimate the content of the reservoir. On the other hand, substantial errors may be introduced in conventional material balance calculations by: (1) the neglect of the amount of oil dissolved in gas at high pressures and temperatures in the reservoir, but which condenses under separator conditions; (2) the assumption that the separation of oil and gas in the reservoir may be duplicated by a differential liberation in the

By R. O. Williams

A recent article by Chernock, Singer, Mueller, and Beck 1 which supports the use of the integral of I sin $ d$ for comparing fiber texture data does not settle what happens to I sin ø as ø approaches zero, where I is the diffraction intensity for poles oriented 0 deg from the fiber axis. They indicate that they believe that it should approach some constant value (that is, I increases without bound) and the fact that in reality it does not was a result of the diffraction

Jan 1, 1960

By A. H. Geisler, R. F. Mehl, C. S. Barrett

The mechanism by which the supersaturated solid solution of 20 per cent silver in aluminum decomposes has been reported in two previous publications.1'2 The analysis of streaks in Laue photograms showed that thin platelike particles (the so-called Guinier-Preston aggregates) form upon matrix planes in the early state of decomposition.1 The size of these particles is larger, the higher the temperature at which they form in accordance with nucleation theory;³ at all temperatures they increase in size with aging.2 When they have grown thick enough to afford three-dimensional diffraction, powder X-ray photograms show that the structure is not that of the equilibrium precipitate but that of a transition lattice . Sincc this is also platelike in shape and also lies upon the (III) matrix planes with the [IIO] direction in the matrix parallel to the [II.O] direction in it seems likely that the original platelet particles are merely in an early stage of formation, and thus finely dispersed. The atomic spacing and pattern on the (00.1) plane in y' are identical with those on the (111) matrix plane to which it lies parallel, and since comparable directions in the two planes are parallel, the lattices are thus coherent at the interface; an analogous coherence has been found in aluminum-copper alloys.3 The structures y' and y are both close-packed hexagonal and are oriented alike; they differ only in interatomic distances. Consequently, y' is regarded as y strained from its ordinary dimensions by the lattice coherency between it and the matrix.2 The lattice movements that transform the matrix to the equilibrium precipitate appear to be very simple.2 The mechanism of precipitation in this system is simpler and is more precisely known than that in any other system hence the system should be a profitable one for the difficult task of correlating property changes with structural alterations. The present report provides additional studies on powder X-ray diffraction from alloys of 10 per cent, 20 per cent and 30 per cent Ag, and presents the correlation of crystallographic changes with changes in microstructurc, Brinell hardness and electrical resistivity of the three alloys. Preparation of Samples and Experimental Procedure The preparation of the 20.2 per cent Ag alloy has been described2 Alloys containing 9.9 and 29.7 per cent Ag were prepared from 99.97 per cent A1 and 99.99+ per cent Ag using a similar procedure. Rolled

Jan 1, 1943

By R. F. Mehl, C. S. Barrett, A. H. Geisler

The mechanism by which the supersaturated solid solution of 20 per cent silver in aluminum decomposes has been reported in two previous publications.1'2 The analysis of streaks in Laue photograms showed that thin platelike particles (the so-called Guinier-Preston aggregates) form upon matrix planes in the early state of decomposition.1 The size of these particles is larger, the higher the temperature at which they form in accordance with nucleation theory;³ at all temperatures they increase in size with aging.2 When they have grown thick enough to afford three-dimensional diffraction, powder X-ray photograms show that the structure is not that of the equilibrium precipitate but that of a transition lattice . Sincc this is also platelike in shape and also lies upon the (III) matrix planes with the [IIO] direction in the matrix parallel to the [II.O] direction in it seems likely that the original platelet particles are merely in an early stage of formation, and thus finely dispersed. The atomic spacing and pattern on the (00.1) plane in y' are identical with those on the (111) matrix plane to which it lies parallel, and since comparable directions in the two planes are parallel, the lattices are thus coherent at the interface; an analogous coherence has been found in aluminum-copper alloys.3 The structures y' and y are both close-packed hexagonal and are oriented alike; they differ only in interatomic distances. Consequently, y' is regarded as y strained from its ordinary dimensions by the lattice coherency between it and the matrix.2 The lattice movements that transform the matrix to the equilibrium precipitate appear to be very simple.2 The mechanism of precipitation in this system is simpler and is more precisely known than that in any other system hence the system should be a profitable one for the difficult task of correlating property changes with structural alterations. The present report provides additional studies on powder X-ray diffraction from alloys of 10 per cent, 20 per cent and 30 per cent Ag, and presents the correlation of crystallographic changes with changes in microstructurc, Brinell hardness and electrical resistivity of the three alloys. Preparation of Samples and Experimental Procedure The preparation of the 20.2 per cent Ag alloy has been described2 Alloys containing 9.9 and 29.7 per cent Ag were prepared from 99.97 per cent A1 and 99.99+ per cent Ag using a similar procedure. Rolled

Jan 1, 1943

By AIME AIME

THE coal classification session* on Monday morning, Feb. 17, was opened by a paper by M. R. Campbell, entitled "Natural Groups of Coal and Allied Fuels," in which he pointed out, by means of graphical presentation of selected proximate analyses of coal, that coals can be classified on the basis of their moisture content. He proposes four groups of coal, brown coal, hydrobituminous, bituminous, and anthracite, each subdivided into two or three sub-groups. In a written discussion of this G. H. Cady, of the Illinois Geological Survey, showed that there is, in general, a progressive decrease in the moisture of Illinois coals from north to south, and that it would be very difficult to draw any arbitrary line dividing the coals of the State into two groups on the basis of moisture content.

Jan 1, 1930

By Rodney P. Smith

The rate of motion of the boundary between a single-phase a-iron region and a two phase a-iron plus ?-iron, or a-iron plus cementite region has been measured on decarburization at several temperatures between 500" and 865°C. These data, together with data for the carbon content of a-iron at the boundary, yield the diffusivity of carbon in a-iron. The activation energy for carbon diffusion is 19.8 kcal per mole for the temperature range —50° to 150°C and increases to an average value of 23.0 kcaL per mole for the temperature range 727" to 865°C. AS part of an investigation of the diffusivity of carbon in iron using a steady-state method,' the diffusivity of carbon in a-iron was determined at the temperatures 802" and 851°C. The diffusion constant thus obtained was larger, by nearly a factor of two, than that predicted from the combined results of stanley2 and of Wert.3 It seemed desirable, therefore, to continue the investigation. Since the temperature range in which the steady-state method can be conveniently used is limited, we have chosen a decarburization method, based on the laws of diffusion in metal accompanied by a phase change.4,5 If the initial carbon content of the Fe-C alloy is such that two phases coexist at the decar-burizing temperature* and decarburization is car- ried out such that the surface is maintained at substantially zero wt pct. C, the carbon distribution after a time, t, will be as shown in Fig. 1. The boundary between the single-phase and two-phase regions moves from y = 0 to y = x in the time, t, where x is proportional4 to tl". If the initial carbon (content of the sample is Ci, and CB is

Jan 1, 1962

By S. A. Lever, R. Hultgren

The solidus is usually the least satisfactorily determined portion of a phase diagram. Cooling curves, which succeed well with the liquidus, show the solidus inaccurately or not at all because of segregation which occurs during freezing. Heating curves of carefully homogenized alloys might be expected to indicate accurately the solidus, but they are seldom used. Dynamic methods involving heating or cooling are never completely satisfactory because of uncertainty as to whether equilibrium is attained. A static method in which the specimen may be allowed hours, days, or even weeks to attain equilibrium is to be preferred. In a static method a solid solution, for example, is first made thoroughly homogeneous, then heated to successively higher temperatures. After sufficient time at each temperature to assure equilibrium, some property is measured which should alter strikingly when melting begins. Microscopic examination can be used to detect the beginning of melting, but the method is tedious since the specimen must be quenched, sectioned, polished, and etched before each examination. Of all the physical properties which change on melting, electrical resistance is probably the most satisfactory to measure. The measurement may be made while the specimen is at temperature without damage to the specimen. It may be repeated indefinitely to ascertain when equilibrium has been achieved. Measurements may be made on a single specimen over the whole range of temperature. Most metals approximately double their resistance on melting. Since an accuracy of a few tenths of a percent is easy to achieve, the method is highly sensitive to the beginning of melting. In spite of these advantages, which have been perceived for a long time,l,2 a reasonable search of the literature has failed to reveal a single case in which the method has been satisfactorily applied in practice to the determination of solidus temperatures. The use of electrical resistance measurements appears to have been confined in practice to changes in the solid state. In the work described in the following pages we have applied the electrical resistance method to the solidus of the lead-tin system. We have found the method to be convenient, reproducible, and highly sensitive. We chose the lead-tin system because it leads to few technical difficulties. Furthermore, a number of determinations of solidus have been made in this system by various methods and results could be checked against them. However, all published results are not in good agreement with one another, so this work should help in determining the solidus more precisely. The Lead-tin Diagram Because of its commercial importance, there have been numerous investigations of the lead-tin diagram. The results of the most recent work on the solidus are indicated in Fig 7, as well as the results of the present work. The works of Honda and Abe3 and of Stockdale4 agree fairly well with each other and with the present work. Jeffery's5 data indicate the solidus to be about 50°C lower. Honda and Abe3 used differential thermal analysis on both heating and cooling cycles. Stockdale4 used the microscopic method and also differential heating curves. Stockdale's results were about 4" higher than those of Honda and Abe at low tin contents and lower at higher tin contents. These results also agree with those of Rosen-hain and Tucker.= Jeffery5 used electrical resistance measurements of the alloy as it was being heated or cooled. Apparently he did not attain equilibrium as his results are about 40°C lower than those of Stockdale4 or Honda and Abe.3 MATERIALS AND METHODS The lead and tin used were of high purity. They were supplied by the American Smelting and Refining Co., who gave the following analyses: Lead: silver, 0.0016 oz per ton; copper, 0.0008 pct; cadmium, 0.0007 pct; zinc, 0.0002 pct; arsenic, 0.0003 pct; antimony, 0.0002 pct; bismuth, 0.0005 pct; tin, 0.0001 pct; iron, 0.0020 pct; lead (by difference), 99.995 pct. Tin: antimony, 0.037 pct; arsenic, 0.020 pct; bismuth, 0.004 pct; cadmium, trace; copper, 0.025 pct; iron, 0.004 pct; lead, 0.020 pct; nickel and cobalt, 0.005 pct; silver, 0.0005 pct; sulphur, 0.005 pct; tin (by .-difference). 99.88 pct. One hundred grams of metal with the desired proportions of lead and tin was weighed out to the nearest one-tenth of a milligram. The mixture was placed in a silica crucible, covered with charcoal, and melted in a reducing atmosphere in a gas-fired furnace. The alloy was well stirred. Chemical analysis of two of the alloys checked closely with the weighed portions. The compositions of the remainder of the alloys were taken directly from the weighings, without chemical analysis.

Jan 1, 1950

By J. J. Gilvarry

Recently, Gilvarry1,2 has given a rigorous derivation of the proper distribution function for fragment size in single fracture, based on a closely defined physical model and deduced strictly by the laws of probability. The physical point of departure is Griffith's theory of brittle strength, identifying sub-microscopic flaws as the cause of the low strength of a solid in comparison with values implied by cohesive energies. Gilvarry and Bergstrom,4-7 and Gilvarry8 have compared the predictions of the theory with experiment, and have found excellent agreement, in general. The purpose of this communication is to sketch the extension of the theory to the case of comminution, and to indicate the applications to some examples in nature. The present treatment represents an amplification of a brief discussion appearing elsewhere. 9 Although the basic ideas of the Griffith theory are perfectly general for rupture of brittle solids, it was originally formulated with very brittle materials such as glass in mind. Moreover, Griffith's original experimental work was carried out on glass specimens. Recently, however, the theory has been extended by race" to apply directly to rocks. This extension makes the theory immediately applicable to the materials generally of interest from the standpoint of comminution. GENERAL CASE To obtain the distribution function for fragment size in single fracture, three assumptions are made, that: 1) Fracture proceeds by activation of preex-istent Griffith flaws in the volume, faces, and edges of a fragment; 2) the distributions of flaws of these three types are independent of each other; and 3) activated flaws of a particular type are distributed at random, individually and collectively, in the sense of Fry.11 The last assumption implies that each distribution is separately of Poisson type.

Jan 1, 1964

By George A. Guess

THE increasing demand for greater speed and more accuracy, in making daily assays of ores and products from mills treating material containing but very small quantities of lead and copper, has caused the older analytical methods to be supplanted by new ones devised to meet the needs of modern work. For " control " work in copper analyses, I had, previous to the present equipment, introduced in my laboratory the ordinary electrolytic method, using hollow cylindrical electrodes, and with these I began a series of experiments in determining the lead-content of daily mill-samples and controls. The results, proving accurate and satisfactory, I then devised, with Mr. H. E. T. Haultain, a cheaper electrode than the ordinary jacket electrode, which costs from $15 to $20,-the expense of the older form making the installation of many units very costly. The form of cathode finally adopted as the most satisfactory, shown in Fig. 1, is cut from 0.001-in. platinum foil. It is 12.5 cm. long, and is divided into a blade 4 cm. wide and 6.25 cm. long, and a tongue 0.7 cm. wide and 6.25 long, the immersion area being 50 sq. cm. and weight 1.5 grams. The blade is first sand-blasted and then corrugated lengthwise, in order to impart the necessary rigidity. Strips of platinum foil 0.001 in. thick, 12.5 cm. long and 0.5 cm. wide, having a median corrugation, form the anodes. Three electrodes are used in each cell, one anode in the middle and one cathode oil each side of the anode. These electrodes are connected to slotted alumi¬num terminals, in which they are held by contact pressure. The terminals are -in. rods, projecting 2 in. horizontally in front of the wall of the cabinet.; at the back the middle electrode (anode) is connected with one pole of the current, and the two outer ones (cathodes) with the other pole.

Nov 1, 1905

By R. E. H. Pomeroy

THE statistical data given in this paper are taken from the actual performance of the No. 2 reverberatory furnace of the Nevada Consolidated Copper Co., Me Gill, Nev., for a period of four months, from April to July, 1914. The principal furnace dimensions are: Length, 132 ft. ½ in. at the skim-line level; average width, 18 ft., 10 in. at the skim-line level. The roof is 7 ft. above the skim-line level at the firing end. The average area in the uptake flue is 36 sq. ft., and the area above the skim line under the vulcatory arch is 24.3 sq. ft. Fig. 1 shows a diagrammatic plan and sectional elevation of this furnace. The furnace is equipped with two 400-b.h.p. Stirling waste-heat boilers set in parallel. California crude petroleum is used for fuel and has a specific gravity of 16.5° B., flashing in open test at 199° F. The oil is heated to about 200° F. in a steam heater before going to the burners, requiring about 9 b.h.p. per furnace day to heat it from the line temperature to the burning temperature. Measurement is made by oil meter, checked daily by reservoir readings. The oil is fed by gravity (34 lb. static pressure) to seven low-pressure blast burners of the Steptoe type (Fig. 2). The blast for these burners is supplied at about 40-oz. pressure by a motor-driven Connersville blower of 42 cu. ft. capacity per revolution. The air supplied by the blower through the burners for atomizing the oil amounts to about 10 per cent. of the theoretical air necessary for complete combustion of the oil. The remainder of the necessary air enters the furnace through the burner openings in the firing wall. No checker holes are provided, and the charge holes in the roof are equipped with slide gates and "dog houses? to minimize air leakages. The combustion of the fuel, as shown by gas analysis at the front of the furnace, is practically complete, the carbon monoxide in the gases being less than 0.5 per cent.

Jan 2, 1915

[Title PAGE 1 Contents Page 1 Officers and Directors5 Standing Committees 6 Professional Divisions7]

Jan 1, 1928

The official Institute reports for the year 1929 were distributed in pamphlet form at the Annual Meeting, February, 1930, and were later included in Section 2 of Mining and Metallurgy, June, 1930, and thus made available to the entire membership. Membership In its report the Admissions Committee set forth the changes in membership during 1929, as follows: Total membership, Jan. 1, 1928, 8582; elected and placed on rolls in 1929, including 59 reinstatements, 509; loss by resignations in 1929, 88; loss by death in 1929, 110; loss by suspension in 1929, 37; membership at end of year not including Student Associates, 8856. Distribution of membership: Honorary Members, 16; Members, 6590; Junior Members, 38; Associates, 1041; Junior Associates, 1033; Rocky Mountain, 138; total membership, Jan. 1, 1930, 8856; Student Associates, 150; total including student associates, 9006. Treasurer's Annual Report, Year of 1929 Statement of Receipts For the year ended December 31, 1929 Dues: Arrears............................................ $ 3,501.75 Current............................................ 97,257.12 New Members...................................... 5,721.50 Advance........................................... 1,970.79 $108,451.16 Initiation Fees.................................................. 7,436.00 Magazine Receipts: Advertising Gross Receipts........................... $40,610.81 Magazine Sales..................................... 3,799.84 44,410.65 Sale of Transactions Current........................... $ 2,985. 15 Sale of Special Editions Current........................ 5,147.82 Sale of Back Transactions and Special Editions........... 4,186.93 Sale of Year Book..................................... 65.50 Sale of Authors' Reprints.............................. 2,585.40 Sale of Pins and Fobs.................................. 14.73 Sale of Technical Publications.......................... 1,451.55 Sale of Bindings...................................... 3,949.13 20,376.21 Net Interest Received: On Bank Balance and Temporary Investments......... $ 2,595.04 On Lie Membership Fund........................... 3,223.43 On James Douglas Library Fund...................... 5,425.61 On General Reserve Fund............................ 2,015.58 13,259.66 Miscellaneous Receipts........................................... 335.80 Total Receipts................................................ $194,269.48

Jan 1, 1930

By Milton F. Goodrich

The idea of using water-only cyclones to scalp clean coal from the feed to other devices has recently been gaining in popularity.l,2,6 An indication of this popularity is that water- only cyclone scalping is already employed in a few commercial plants. Water-only cyclones scalp the feed to a heavy media vessel in the Warwick plant,3 to Deister tables in the Rowland plant,4 and to a heavy media cyclone circuit in the Amherst Coal Company's McGregor plant.5 Despite this trend, we found surprisingly little information in the literature on the performance of water-only cyclone scalping. Therefore, we undertook a study of its technical merits, limiting our investigation to a water-only cyclone scalper in conjunction with heavy-media cyclones. We felt this to be a reasonable combination of equipment, since both processes operate well on the same size coal. First, we developed simple mathematical relationships revealing general characteristics of the system. Next, we compared the clean coal yield and quality obtainable by the system on four different coals with that obtainable by heavy-media cyclone circuit alone and water-only cyclones middlings recirculation circuit alone. This was done by using computer program to simulate the operation of the three systems. Finally, we considered the effect that implementation of the system would have on a typical preparation plant circuit.

Jan 10, 1978

The Library of the above-named Societies is open from 9 A.M. to 10 P.M., except on holidays. It contains about 70,000 volumes and 90,000 pamphlets, including sets of technical periodicals and publications of scientific and technical societies. Members of the Institute, with few exceptions, are forced to spend a portion of their time in localities isolated from sources of information. To these the Library, through its Library Service Bureau, can render valuable service through correspondence; letters requesting information will receive especial attention. The Library is prepared to furnish references and photographic copies of articles on mining and metallurgical subjects; to determine the existence of mining maps, and to furnish general information on the geology and mineral resources of all countries. All communications should be made as definite as possible so that the information received may be what is desired and not include collateral matter which may not be of interest. The time spent in searching for such collateral matter will be saved, and the information will he sent more promptly and in more usable shape.

Jan 9, 1917

By J. B. Hiskey, W. J. Schlitt, W. G. Pitt

Aqueous SO2 (sulfurous acid) is an interesting chemical compound. It functions as a reagent in various hydrometallurgical systems, but also represents an undesirable constituent in gyro- and hydrometallurgical effluent solutions. When present in such streams, SO2 can be oxidized to the more stable sulfate form to avoid exsolution of SO2 as a source of fugitive emissions and to simplify standard water treatment plant operation. This study provides information on the stoichiometry, kinetics, and mechanism of SO2 oxidation using oxygen and an iron salt catalyst with solutions containing 0.05-20 g/L (0.002-0.7 oz per gal) SO2. The effects of iron salt concentration, oxygen pressure, temperature, degree of agitation, and pH on SO2 oxidation are also described.

Jan 1, 1984

By E. R. Helderman, C. Y. Ang, C. C. Nealey

Beryllium-base alloys have been successfully p7.-epared by the liquid-phase sintering technique. Depending orz the composition and amount of the intended liquid please, microstructures either single -phase or duplex in feature with randomly oriented grains have been obtained. Qualitative and semi-qualitative determination of distribution of alloying elements md microsegregations in some experi)uzental alloys haue been made by electron-micro-probe analysis in conjunction with microliardness testing and standard metallography. Tensile tests reoealed that some conzpositions possess attractive elastic properties with Young's mot1uli greater than 40 X 10' psi. In powder metallurgy, liquid-phase sintering is a process or phenomenon that has proven to be of practical value. For example, the heavy metals such as tungsten-copper-nickel, high-strength heavy gyro alloys,' heavy-duty electrical contacts,' and tungsten carbide tool materials are all products of liquid-phase sintering. Mechanisms involved in liquid-phase sintering, however, are not completely understood. Questions regarding the exact roles played by rearrangement of particles, liquid/vapor surface energy, solution and precipitation, and so forth, have not been completely answered. Evidence has been cited3 that at least volume shrinkage in the densification process is diffusion-controlled. It is possible that the predominant mechanisms for the complete densification and grain growth in a liquid-phase sintered system depend primarily on the alloy systems involved, in addition to processing conditions. Despite the lack of sound understanding of the mechanisms of the process, liquid-phase sintering has been and is being used to advantage either to synthesize microstructures for their special properties or to prepare alloys which are difficult to form by fusion process. Liquid-phase sintering of beryllium alloys was first attempted by Jones and Williams.4 They first tried infiltrating beryllium with magnesium, and then succeeded in preparing the alloy by sintering Be-Mg powder compact in molten magnesium bath. This investigation resulted in the identification of some Mg-Be intermediate phases. Crossley et a1.5 also used liquid-phase sintering technique in an attempt to produce ductile beryllium alloys for structural applications. The major liquid-phase components investigated by Crossley et al. were aluminum and silver with minor additives of germanium, calcium, lanthanum, cerium, and yttrium. The lack of wetting and the bleeding out of liquid phase were the difficulties encountered during experimentation. According to Hodge,6 the two compositions investigated by Crossley, which showed some promise based on compression tests, involved large amounts (over 35 wt pct) of silver, thus making them too heavy to be of practical interest to the aerospace industry and military users. The present investigation was prompted by the search for light-weight (density less than aluminum) beryllium alloys exhibiting small anisotropy in physical properties for precision inertial navigation instrument applications. In addition to isotropy, good structural properties such as high elastic modulus or desirable combination of mechanical and physical properties are also objectives of this investigation. The technique of liquid-phase sintering was chosen for its versatility in producing either duplex or homogeneous microstructures. This report is concerned with the use of copper and aluminum, with or without silicon addition, as the intended liquid phase, and the resultant micro-structures and some physical properties of the beryllium alloys. Qualitative and semiquantitative electron-microprobe analyses of some of the alloys are presented to illustrate the usefulness of this microanalytical technique for the identification of microconstituents and their distribution. EXPERIMENTAL PROCEDURES The beryllium powder used was -200 mesh Brush Beryllium Co. QMV NP-50 grade. Typical chemical analysis of the powder is shown in Table I. Commercial high-purity copper, aluminum, and silicon powders all screened to —100 mesh were used as additions. Mixed powder compositions were ball-milled in ceramic jars for 1/2 hr to ensure thorough blending. Milled powder was loaded either in 3/4-in.-diam button die or in Metal Powder Association flat tensile specimen die and compacted under top and bottom pressure. No lubricant or organic binder was used. Sintering was carried out in a quartz tube under a vacuum of 50 to 100 µ pressure. Surface hardness and some microhardness readings were taken on sintered specimens. Sintered density was

Jan 1, 1965

By A. J. Jacobs, G. Katz

MANY of the studies of intermetallic compounds containing uranium were performed during the early 1940's under the aegis of the Manhattan Project. Subsequently, much of this work was declassified and published after 1949. In some instances this early work, completed with relatively impure materials, represents the only source of X-ray diffraction powder data available in the literature. In the case of the intermetallic compound U,Fe some discrepancies in the powder pattern exist in the literature. Since this compound has been prepared in this laboratory, it is believed that the publication of the indexed powder pattern would help clarify the conflict in the literature. In studies of the U-Fe system, Gordon and Kauf-mannl and Grogan and Clews2 independently reported the intermetallic compound U,Fe in 1950. The crystal structure was described by Baenziger, Rundle, Snow, and Wilson3 in 1950. It is isostructural with U,Mn, U,Ni, and U,Co and crystallizes in a body-centered tetragonal lattice. The lattice constants determined by Baenziger et al. are: giving an X-ray density = 17.7 g cm-3 for 4 mol per unit cell. The compound used in this study was prepared by melting a stoichiometric mixture of the constituent metals in an argon-arc furnace using a nonconsum-mable tungsten electrode. Before the argon of 99.98 pct purity was introduced into the furnace, it was passed through CaC1, to remove water vapor and afterwards through a stainless steel tube containing calcium turnings heated at 600°C for the removal of nitrogen and oxygen. The purity of the uranium used was better than 99.9 pct and that of the iron was 99.97 pct. Before and during melting a zirconium getter was used to further purify the argon atmos-

Jan 1, 1962

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who called at Institute headquarters during the period Apr. 10, 1916; to May 10, 1916: Philip P. Baily, New York, N. Y. George W. Otterson Seattle, Wash. John M. Brooks, Jr., Knoxville, Tenn. C. Q. Payne, New York, N. Y. C. A. Burdick, New York, N. Y. Charles F. Potter, Los Angeles, Cal. W. N. Crafts, Oberlin, Ohio. Albert E. Rhoads, Harrisburg, Pa. Andrew B. Crichton, Johnstown, Pa. M. F. Sayre, Schenectady, N. Y. 0. P. Hood, Pittsburgh, Pa. H. V. Smythe, Northpines, Ont., Canada. W. McA. Johnson, Tulsa Okla. W. 0. Snelling, Long Island City, N. Y. G. H. Morgan, New York, N. Y. W. H. Staver, Ophir, Colo. E. G. Norton, Chicago Ill., A. W. Tucker, Salisbury, N. C. M. L. O'Neale, Coal City, Ala. Andrew Weisenburg, Philadelphia, Pa. Arthur H. Brown has resigned his position with the Dome Lake Mining & Milling Co., South Porcupine, Ont., Canada. Robert Sterling has resigned his position as chief engineer of the Goldfield Consolidated Mines Co., Goldfield, Nev., to accept the position of assistant manager of the vanadium mines of the Primos Chemical Co., Vanadium, Colo.

Jan 6, 1916

By O. N. Carlson, S. A. Bradford

Discontinuous yielding in tensile tests was observed in V-O alloys in the temperature ranges of 150° to 175°C and also 350° to 400°C. The magnitude and intensity of the serrations were found to vary considerably with oxygen content. Maxima were observed in tensile and yield strengths and in the strain-hardening coefficient at the higher temperature only. The strain rate sensitivity was observed to be negative between 150° and 400°C. THIS investigation was undertaken to study the effect of oxygen on the tensile properties of iodide vanadium in the temperature range of 25o to 450°C. Brown1 observed an increase in strength between room temperature and 400°C in vanadium metal, and found that oxygen and nitrogen had a rather pronounced effect on the strength and ductility. A maximum in the tensile strength was observed by Rostoker et al.2 near 300oC and by Pugh3 around 450°C for calcium-reduced vanadium. Pugh also found a maximum in the yield strength and in the strain-hardening exponent, and minima in the elongation and strain rate sensitivity at the same temperature. Eustice and Carlson4 reported the appearance of serrations in the stress-strain curves between 140° and 180°C in iodide vanadium containing 600 ppm O. These anomalies in the mechanical properties indicate that strain aging occurs in vanadium, but the impurity or impurities responsible for the above-mentioned effects have not been identified. The phenomenon of strain aging is usually characterized by the return of the yield point after interruption of a strength test. In the temperature range where strain aging occurs, the yield and tensile strengths attain maximum values, elongation and strain rate sensitivity exhibit minima, and discontinuous yielding is generally observed in the stress-strain curve. Cottrell5, 6 has postulated that strain aging is due to the migration of solute atoms to dislocation sites to produce locking after the dislocations have broken free from their impurity atmospheres during the initial yielding. At the strain-aging temperature the process is a dynamic one in which the solute impurity atoms diffuse to the vicinity of the moving disloca- tion producing "locking" which gives rise to maxima in the tensile strength and serrations in the elongation curves. Cottrel17 has noted that discontinuous yielding in iron occurs when the diffusion coefficient of nitrogen, D, and the strain rate, i, are related by D = 10-9 €. EXPERTMENTAL PROCEDURE The vanadium metal employed in this study was prepared by the iodide refining process as described by Carlson and owen.8 A representative analysis of the vanadium used in this investigation was: 150 ppm O, <5 ppm N, <1 ppm H, 150 ppm C, 150 ppm Fe, 70 ppm Cr, <50 ppm Si, 30ppm Cu, 20 ppm Ni, <20 ppm Ca, <20 ppm Mg and <20 ppm Ti. Alloys containing from 200 to 1800 ppm O, all of which lie in the solid solution range of the V-O system, were prepared by arc melting vanadium together with portions of a high-oxygen master alloy. The master alloy was prepared by tamping pure V2O5 into holes drilled in a vanadium ingot and arc melting this five or six times in an inert gas atmosphere, inverting the button between each melting step. The oxygen content of the master alloy was then determined by vacuum fusion analysis. Vanadium containing less than 150 ppm O was prepared in the following manner. A bar of iodide vanadium was deoxidized by sealing it in a tantalum crucible with a few grams of high-purity calcium. This was held at 1100°C for 4 days to allow time for the oxygen to diffuse to the surface and to react with the calcium vapors. The calcium oxide product was later dissolved from the surface of the bar with dilute acetic acid. In this way vanadium containing from 20 to 50 ppm O was prepared. Sample Preparation. The are-melted ingots were cold swaged into 3/16-in. diam rods and these were machined into cylindrical tensile specimens with a reduced section of 1.00-in. length and 0.120-in. diam. The test specimens were annealed for 4 hr at 900°C in a dynamic vacuum of mm of Hg to remove hydrogen from the metal. This recrystal-lization treatment produced a uniformly fine-grained structure with a mean grain size of approximately 0.06-mm diam. The oxygen contents reported in this paper were determined by a vacuum fusion analysis of the tensile specimens after testing. Analyses for other interstitial or metallic impurities showed no significant changes from that of the original material. Tension Tests. Tension tests were performed on a screw-driven tensile machine at a constant cross-head speed of 0.01 in. per min. Tests at elevated temperatures were carried out by heating the

Jan 1, 1962