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By Herbert Hoover

DURING the year, the' Institute has made the most remarkable growth in its history. Our actual increase in membership was 1816 and therefore was 80 per cent. larger than any previous year. Even without expectation of any abnormal growth, we should pass in the year 1921 the 10;000 mark. The causes of this increased growth are not far to seek.. They lie in the widening vision of the Institute's work, not only in its relation to' the profession but as an avenue of service to the nation as a whole. The Institute is today in the first rank of influence among public institutions in the country. During this year we have, for the first time in many years, had a ?deficit of some $3000 in our finances. The sum is not important, but it- does indicate the tendency of the times, and that is the high cost of living:' The increase in our expenses lay, to the largest degree, on the publishing side of the Institute's work. If we compare the year 1918, as a fairly repre¬sentative year, with that of 1920, we find that the costs of issuing the' Institute's publications, after deducting the income received from these publications, shows a .net increase of about $33,000. for the year. This has been to some degree due to the enlarged membership but to a large degree due to the cost of the paper and printing.

Jan 1, 1921

Jan 1, 1969

AALL,Christian H.,(M '49), Asat.Research Dir , Phosphate Div Monsanto Chem.Co.,Monaanto, Tenn. AAMOT,Olav Crone, (M '29), Dir of Tech., Chromium Min. & Smelt. Co Ltd Box 6215, Hillyard, Spokane, Wash. AARING, Floyd Daniel, (J '48), Prod. Engr., Canadian Gulf Oil Co., 8035 - 102nd St., Edmonton, Alta., Canada AASE, Glenn D., (J '40), Met Engr Western Research Div. ,Amer. Smelt. & Refin. Co., Selby, Calif ABADIE, Henry G (M '43), Senior Prod Engr., Long Beach Oil Dev Co., 255 S Santa Clara Ave Long Beach 2, Calif. ABBOTT,Clarence E (M '04), Civil Engr., 901 Insurance Bldg., Raleigh, N.C. ABBOTT, John, H., (M '46), Resident Mgr., Hickman, Williams & Co., Rm 2205,230 N Michigan Ave., Chicago 1. I11.

Jan 1, 1952

By B. A. Kulp, R. R. Reeber

Lattice parameters for the wurtzite form of' CdS mere measured by powder X-ray diffraction techniques over the temperature range 26° to 1000 K'. A negative thermal -expansion coefficient was determined parallel and perpendicular to the c axis below 13.5°K. Near 808°K, the curves of the a, parameter, the differential thermal expansion, and the resistivitv vs absolute temperature exhibited a reversible discontinuity. j\. direct determination of the lattice parameters of CdS over an extended temperature range is of particular use in interpretation of the effects of high pressure on the band structure of semiconductor materials. For example, Langer' has studied the effects of pressure on the absorption edge of CdS from 77°K to room temperature. In order to properly interpret his results it is necessary to know the change in lattice constants as a function of temperature for the wurtzite, zincblende, and rocksalt2 modifications of this material. Thermal-expansion measurements for CdS, wurtzite phase, have previously been determined over a limited temperature range.s74'5 The zincblende phases, of other compounds with similar bonding, have been investigated by Novikova et a! .'' Previous thermal-expansion measurements for metals with hexagonal symmetry have for the most part used bulk sample techniques for low-temperature result. Most X-ray measurements at low temperature have been on materials with cubic symmetry.'jQ The use of X-ray powder-diffraction techniques offers a convenient and accurate method of measurement over a wide temperature range. The X-ray method, besides measuring unit cell size, also provides information about change in structure type and the nature of some of the stacking defects present. I) EXPERIMENTAL PROCEDURE The thermal expansion was measured by X-ray powder-diffraction techniques. Lattice parameters for the range 300" to 1000°K were determined in a 19-cm Unicam camera. From 26" to 300°K a 34-cm back-reflection camera with the Van Arkel" film arrangement was used. The sample was bonded to a copper cold finger below a helium, hydrogen, nitrogen, oxygen, dry ice, or ice brine bath in a metal cryistat. che inner bath was surrounded by another one for radiation shielding. Nitrogen was used in this outer bath for the very low-temperature runs while dry ice and acetone was used for the 195°K point. CuKa X-rays, filtered with a nickel foil, entered the cryostat through a 0.001-in.-thick aluminum window. During a typical 9-hr exposure the sample was continuously rotated through a 30-deg arc. Heat losses from the sample holder limited the minimum temperature attained to 26°K with helium in the inner dewar. Temperature calibration between 25" and 125°K was determined with an Allen Bradley 300-ohm carbon resistor. The resistor was attached to the back of the copper finger with a thin layer of silicone grease. Liquid He, HZ, N2, and O2 baths were used to calibrate the resistor. Temperature variation is estimated to be *2"K with a slightly higher uncertainty at room temperature and 264°K. The thermal expansion of high-purity germanium from 373" to 900°K was measured as a calibration for the Unicam camera. This value was compared with the known value1' for the thermal expansion. A discontinuity in the thermal-expansion coefficient of the CdS a, parameter was observed. Similar discontinuities in the resistivity and differential thermal analysis at the same absolute temperature indicate that the temperature error is *5°K in the temperature range above 500°K. Temperature errors in the Unicam camera below 500°K are appreciably higher due to large gradients in the resistance furnace. II) SAMPLE PREPARATION The CdS was Eagle Picher ultrapure grade. The crystallite size range of the as-received powder

Jan 1, 1965

Organization Place Date 1919 American Chemical Society Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters' Society, First Annual Convention Chicago, 111. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, O. Sept. 29-Oct: 2 American Foundrymen's Association Philadelphia, Pa. Sept. 29-Oct. 4

Jan 9, 1919

By K. H. Heino

Two 200 T/da Lurgi Turbulent Layer fluid-bed roasters have been in operation at Canadian Electrolytic Zinc Limited since 1966. Zinc concentrate containing 52-54% Zn, 9-11% Fe,31-33% S is treated to produce calcine containing 60-62% Zn,10-12% Fe, .l-.3% S as sulphide and .8-1.2% S as sulphate. Each roaster train comprises a waste heat boiler, two cyclones in parallel and a two-field electrostatic precipitator. Distribution of calcine collected is 10-15 percent from bed overflow, 55-65 percent from boilers, 20-25 percent from cyclones and 2-6 percent from precipitators. A Monsanto designed contact plant produces acid at a rated capacity of 365 T/da (100% H2304 basis) from roaster gases diluted to 7.0-7.5% S02. The process steps are gas cleaning and cooling by weak acid scrubbing, acid mist removal in electrostatic precipitators, gas drying in 93.5-96.5% H2304, conversion of sulphur dioxide to sulphur trioxide in a four-pass converter containing vanadium pentoxide catalyst, and absorption of the sulphur trioxide in 98.1-98.3% H2S04. Product acid is 93.2% H2S04. Conversion efficiency is 97-98 percent and overall sulphur recovery from concentrate is 87-90 percent. The adjacent fertilizer plant has a capacity of 135 T/da of P205. The products are 54 percent phosphoric acid, run-of-pile triple superphosphate, and diammonium phosphate. The plant is of Ugine-Kuhlman design and consists of an air-cooled multiple tank reactor, a tilting pan filter, and a forced circultation vacuum evaporator. Triple superphosphate is made on a continuous belt and partially cured in a rotary dryer. Diammonium phosphate is produced by ammoniating phosphoric acid in a single stage reactor. The slurry of ammonium phosphate is granulated in a blunger and dried.

Jan 1, 1970

By S. F. Emmons

Jan 1, 1899

By T. Kunitake, H. W. Paxton

The self-diffusion coefficient of chromium in various alloys in the iron-chromium system has been measured. A variation in Dofrom 10-4 for pure chromium to a maximum of 102 near 60 pct Cr appears with a range of activation energy from about 50 to 80 kcal per mol. The general pattern of behavior observed is not consistent with present theories of diffusion by a vacancy mechanism. Suggestions are made for further clarifying experiments. RECENT work on the self-diffusion of chromium,' ?-uranium2-4 and ß-zirconium,23, 26 has indicated that these elements have very low Do (10-3 to 10-4) compared to that conventionally expected for vacancy diffusion. Pound et al.5 have suggested that this may be due to ring diffusion being operative, and have proposed a model which gives Do of the correct order of magnitude. The essential difference between this model and Zener's earlier model6 is that whereas Zener assumes tight coupling between atoms in a ring to establish a vibrational frequency, Pound's model allows the atoms to vibrate essen- tially each in their own normal modes. The probability of each atom moving in the correct direction to cause a ring of n atoms to rotate by 2p/n must then be calculated as a "synchronal entropy" which may be -20 e.u. for a 4 atom ring. In iron, the latest determinations of self-diffusion yield Do in the range 18 to 522.7-9 The most accurate is probably that of Borg and Birchenall8 which is 118 ± 3. This value is not inconsistent with that expected for a vacancy mechanism. Since iron and chromium are very closely similar in size, are both transition metals, and their solution is thermodynamically ideal at temperatures of interest in diffusion, it appeared that a determination of self-diffusion coefficients, Do and Q as a function of composition would be of substantial interest to diffusion theory. The following measurements were made with this purpose in mind.

Jan 1, 1961

By K. G. Gorling, S. J. Wallden, N. B. Lindvall

It is the policy of The Metollurgical Society to provide, in the TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AIME, a prompt and accurate medium for publication of reports of significant new research in both the scientific and engineering aspects of metallurgy. Papers submitted to the Society are judged by competent reviewers according to established criteria for technical merit, accuracy, originality, and presentation. STAFF: Editorial Director, Rixford A. Beals; Associate Editor, James J. Burke; Assistants, L. Capria and R. K. Larkin. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: A. W. Thornton, Choirmon; Dennis Carney, John Chipman, J. C. Fulton, J. H. Hollomon, H. tl. Kellogg, A. E. Lee, R. Maddin, J. D. Sullivan, and O. Swan. Review and selection of manuscripts is under the supervision of the following Publications Committees: Extractive Metallurgy Division T. B. King. Cha~rmon; S. J. Dickenson, R. P. Hermsdorf, R. Schuhmann, Jr.. and P. T. Stroup. Institute of Metals Division: Robert Maddin, Chairman. F. Lincoln Vogel, Jr., Vice-chairman, W. A. Backofen, R. W. Balluffi, J. H. Bechtold, M. B. Bever, R. S. Busk, C. G. Goetzel, Paul Gordon, C. D. Graham. Jr., Robert F. Hehe-mann, R. I. Jaffee, F. E. Jaumot, Jr., lrving R. Kramer, A. J. Leno, Horold Margolin, C. J. McHorgue, Russell A. Meussner, J. 6. Newkirk, H. W. Paxton, G. E. Pell~ssier, I. S. Servi, Alan U. Seybolt, A. J. Sholer, and Sack Wahsburn. Iron and Steel Division: J. C. Fulton, Chairman; T. B King, F. C. Langenberg, W. O. Philbrook, and T. B. Winkler. Published bimonthly by the American Institute of Mining Metallurgical and Petroleum Engineers Inc., 29 West 39th Street, New York 18, N. Y. Telephonne pennsylvania 6-9220.Petroleum Subscription Engineers$20 per year for non-AIME members in United States and North South and Central 6-9220.SubscriptionAmerica $25 toreign; $5 for AIME members. Single copies, $4.00, iinalo copies Southfpr;ign,andCentral $5 00. The AIME 'is $25not responsible for any statement made or opinion expressed in its publications Copyright 1958 1958 by the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . Registered coble address, AIME New York . . . Indexed in Engineering Index, Industrial Arts Index, ...and Chemical Abstracts . . . Application for second class mail privileges IS pending at New Yark, N. Y. Volume 212, Number 2.

Jan 1, 1959

By C. R. Kuzell

IN COMPARISON with recent years 1932 has yielded much less tangible evidence of progress in copper reduction and refining. The industry has been extremely quiet, especially in the United States. Design and construction has been throttled by lack of new capital expenditures. The excess producing capacity of the whole industry and the extremely gloomy outlook for the future have made it unwise to tie up more capital except under special conditions. The plants built during the previous year have, however, been placed in operation. Older plants have been abandoned, temporarily shut down, placed on part time operating basis, or continue to operate at a low percentage of normal capacity. In the United States the Phelps Dodge Corporation at Douglas, Ariz., has completed the remodeling of the former Calumet & Arizona smelter. A new roaster and Cottrell plant chimney was completed this year. Though operations have been limited the new equipment has been found to justify all expectations. The reverberatory plant addition consists of two furnaces 26 by 107 ft. inside dimensions, with a high arch, and modern steel binding of excellent design. Natural gas fuel gives good results. One of these furnaces will treat 1000 tons of solid charge per day with a fuel consumption of approximately 3,000,000 B.t.u. per ton. The larger converters have not only yielded the expected lower costs, but have simplified operations in the converter department. One of the noticeable results is the greater cleanliness in the environment and the absence

Jan 1, 1933

Jan 1, 1970

By H. Linder, W. H. Dennen

The graphitic carbon content of soils may be used to detect and delimit subsurface graphitic zones. Spectrographic measurement of carbon in C horizon soils from several areas in the northeastern United States shows good correlation with known graphitic bodies. Bodies of graphite and sulfides are readily located by electromagnetic prospecting methods, but these methods cannot generally discriminate between them. Usual practice, therefore, requires follow-up work on electrically anomalous areas by trenching, drilling, or soil sampling in order to determine the mineralogical nature of the conductor. The efficiency and cost of such follow-up is consequently an important factor in prospecting. The presence of buried sulfide deposits is often reflected in concentrations of metals in the superincumbent soil. Simple chemical tests for such metal concentrations have been developed and applied with considerable success. Bodies of graphite or mixtures of graphite and sulfides are, however, very common and a means whereby buried graphite could be detected by soil testing should provide valuable additional information in the search for ore sulfide and graphite deposits. Graphite is a notably stable substance and should persist in soil above graphite-rich horizons. Microscopic examination of soil samples high in carbon, however, failed to reveal any recognizable graphite fragments indicating a grain size in the clay range. Presumably such small particles would have some mobility in a soil by a translocation mechanism similar to that proposed for the movement of clay particles in a soil profile. Experimental data supports this idea since the boundary between background and anomalous soils carbon values is quite sharp, but the anomalous zone is slightly broader than the graphitic source rock. A simple spectrochemical technique for the determination of carbon in geological materials has been described by Dennen,1 and may be directly applied to soils. A modification of this technique which employs an arcing chamber through which nitrogen is passed is recommended to decrease contributions from atmospheric carbon dioxide. Tests indicate that soils over graphitic zones may be strongly enriched in carbon. The spectrochemical determination of carbon depends upon the formation of the cyanogen molecule (CN) from carbon in a sample and atmospheric nitrogen, under the high temperatures associated with a dc arc. Samples for analysis are dried, lumps broken, and screened. A small portion of the -100 mesh fraction is packed into a copper electrode and excited as the cathode of a dc arc. The band spectra of cyanogen are recorded photographically and the density of the bandhead CN 3883A is measured. The limit of detection of the method is about 0.01 pct C and its coefficient of variation is about 15 pct. Soils, of course, contain carbon in other forms than graphite, and the amount of interference from such sources was examined. The C horizon of several soils from Massachusetts, Maine, and Pennsylvania were found to have a carbon content of 0.3 to 0.5 pct by weight. This content is chiefly due to the presence of carbonates and vegetable matter in the sample and may be readily eliminated, or at least

Jan 1, 1961

By H. K. VAN POOLLEEN, W. Hurst, H. C. Bixel

In an earlier publication* I showed the development of the instantaneous point source solution for a well producing at a constant rate at the center of a system of two radial, adjoining sands of different permeabilities. I also showed how a wellbore radius could be incorporated if this were the development required. For the purpose of that paper and the point I wished to make, this solution served. It yielded a simplifying solution of sands in series identified by Eqs. VI-26 and VI-27. (These equations are reproduced in part by Bixel and van Poollen as their Eq. 3, Page 302.) I am well aware that the simplified solutions are approximations. The facts that these Ei-functions satisfy the diffusivity equation and meet the boundary conditions both at the well and at the interface between sands, and that the earliest time considerations yield zero pressure drop, are evidence that the solutions are good approximations. This was the purpose for these formulas, which I interpret that where the permeabilities are of finite order of magnitudes in the respective media, the relations give satisfactory answers. However, from the authors' point of view there are reservations, which leads me to consider their entire generalization as illustrated in their Figs. 1 through 14. What I understand from their storage capacity, relationship Fs, which is the ratio of the product of porosity and compressibility of Sand II to Sand I, that is employed here by the authors as a correlative means of identifying one figure from another, there is nothing in the exact mathematics that supports such a term as a means of correlation. This is taken out of context, unsustained that this applies. Here the mathematics are known, where the true correlation is the diffusivity term of one sand to another. This entails permeability that refers back again to the term M in their paper for the transmis-sibility of fluid from one sand to the other that should have also been a part of this storage capacity. In Figs. 8 through 14, which purported to show the simplified equation following this correlation, there are apparent discontinuities for M equal to or less than 0.1000 that differ from the trends for greater values of M. In this connection there is no reference radius given for this cumulative pressure drop in the paper that would permit me to make these calculations. However, what is clear for M equal to 0.1000 or less we are treated to almost a closed barrier at the interface; a condition entered by the writers without qualification. This across-the-board treatment of these simplified formulas, whatever the motive of the authors, enters into a range of permeabilities that even I as the contributor would have reservations that such could apply. Under comparable conditions I would be looking at a closed reservoir or some facsimile for such. The extent to which the approximation or the exact equations pertain is not evident in the generality offered by Bixel and van Poollen in their paper. Only when they or other writers show the comparison of the pressure distributions within the formations can one be able to judge the rational limits to subscribe to the simplified formulas.

Jan 1, 1969

By Herbert Hoover

BOTH the directors of industry and your leaders have made great progress toward a new and common . ground in economic conceptions, which, I am confident, has had a profound effect upon our economic progress during the last few years. That is the conception that industry must be constantly renovated by scientific research and invention; that labor welcomes those labor-saving devices; that labor gives its full and unrestricted effort to reduce costs by the use of these machines and methods; that the savings from these reduced costs shall be shared among labor, employer and the consumer.

Jan 1, 1930

By Robert Pack

INTRODUCTION SOONER or later in the development of any natural resource it becomes highly desirable to know the quantity of this resource in the country as a whole, as well as of the part that is being developed, for the general course and. conduct of the development work must be governed to some extent by the total supply available. An accurate estimate of the quantity of any natural resource is difficult to make; yet if one is diligent enough one can obtain a pretty accurate idea of the quantity of marketable timber, the acreage of tillable land, or the horsepower that may be developed from the streams, for these are things that may be measured. But any attempt to estimate the quantity of some mineral in the ground appears to enter the realm of imagination and it seems that the estimate can be nothing more than a blind guess. It may appear to be especially futile to attempt to determine the quantity of oil and gas that is available in the ground, for these minerals are so vagrant that even if the quantity now available should be known quite exactly, the quantity that will eventually be obtained may be much less, for certain losses in the extraction of both oil and gas are unavoidable, and just what these losses will be cannot be predicted. Though necessarily inaccurate, estimates of such mineral reserves are, however, of distinct value, for they summarize the existing knowledge of the deposits of the mineral and thus enable those who are interested in some industry that depends in one way or another on this mineral to formulate a rational commercial policy. Some time ago, when the price of gasoline suddenly rose in a rather spectacular manner, the writer was one of the U. S. Geological Survey geologists called upon to help to estimate the quantity of oil that could be obtained in the United States, for the fear had become widespread that perhaps the rate of increase in the price of gasoline was a measure of the rate of depletion of the supply of petroleum. It thus became his

Jan 8, 1917

Institute of Metals Division Ferrous and Nonferrous Physical Metallurgy Established as a Division April 26, 1918 (Bylaws published In the 1944 TRANSACTIONS Volume of the Division) A A SMITH, JR, Chairman E A ANDERSON, Past-Chairman F N RHINES, Senior Vice-Chairman W A DEAN, Vice-Chairman H A MALONEY, Treasurer ERNEST KIRKENDALL, Secretary 29 West 39th Street, New York 18, N Y Executive Committee R M BRICK 2 W A JOHNSON 1 H I DIXON 2 E W PALMER 1 M GENSAMER 2 J H SCAFF 3 J D HANAWALT 1 J D SULLIVAN 3

Jan 1, 1952

By W. T. Bell, M. P. Lebourg

The perforating of multiple tubingless completions, in which two or more strings of 27/8-in. OD casing are installed in the same borehole, presents two basic problems. First, good completion practices require an eficient perforator that leaves no debris to interfere with subsequent completion operations. Second, and of more complicated nature, a system is needed for controlling the direction of fire so that adjacent strings are not damaged. Development of of a 2-in. OD, steel retrievable, shnped-charge gun has solved the first problem. The second was resolved through development of three different devices to provide directional perforating for the two types of completion methods being employed today. These include a mechanical orienting device and two self-orienting radiation devices. Conceivably, the latter methods could be adapted to the directional perforating (of .upper zones) of conventional dual and triple completions without removing production tubing and packers. INTRODUCTION The recent trend to multiple tubingless completions,' wherein two or more strings of 27/8-in. OD casing are installed in the same borehole, has presented two basic perforating problems. The first problem to be overcome was the design of a gun that would result in efficient perforations without causing debris to bridge in these small-diameter casings. The second problem was, of course, to devise a system for controlling the direction of fire such that adjacent strings would not be damaged. The problem of gun debris in slim-casing completions has been well defined in the numerous 27/8-in. single tubingless completions which have been effected during recent years with the expendable-type perforators. Failure of expendable-gun debris to settle out properly, even with good gun break-up, has resulted in bridging inside these small-diameter casings. This, in turn, has interfered with completion and re-conditioning operations. The past two years have clearly shown, in fact, that debris problems are not confined to this small range of casing with most designs of expendable-type guns. A high incidence of bridging has even been reported in 4%-in. OD casing. The perforating of multiple tubingless completions has entailed, therefore, the development of a completely debris-free gun of adequate performance, as well as the necessary devices to provide positive directional perforating in the two completion methods presently being employed. THE GUN —DESIGN CONSIDERATIONS The design of a shaped-charge gun for slim-casing perforating has presented a maze of interrelated prob-lems. Since the primary specification has been leveled at efficient charge performance with complete elimination of gun debris, it has been necessary to develop a retrievable steel-carrier gun of tubular construction to house the charges. The carrier must be retrievable through 2.29-in. API pump-seating nipples which are usually installed in 2 7/8-in. strings. To provide for recovery of the gun from the well, swelling of the carrier on firing must be carefully controlled. Control of swelling automatically means control of explosive weight in the shaped charge which, in turn, influences charge performance. Carrier swelling also depends upon the confinement pressure at the level being perforated, which imposes a hydrostatic pressure-depth limitation. Burr interference on the wall of the carrier, resulting from passage of the jet through the carrier wall, must be eliminated by suitable design. Clearly then, a satisfactory shaped-charge gun design for slim-casing operations represents a fine balance between carrier swelling, hydrostatic pressure, explosive weight and charge performance. Additionally, to lend itself to directional perforating, the gun design must provide a positive locking mechanism for individual charges within the gun carrier. This fixes charge orientation within the carrier and prevents

By B. Wilshire, P. W. Davis

It has been shown that grain-boundary migration during high-temperature creep can reduce or even prevent the formation of intercrystalline voids, giving a considerable increase in ductility.' A similar observation has been made in a recent investigation of the creep properties of various grades of nickel and nickel alloys. The results can be illustrated by the observations made on: a) Pure vacuum-cast nickel (99.993 pct Ni) b) Impure vacuum-cast nickel (99.97 pct Ni) c) Pure nickel containing internal voids (produced by a process of intering). d) A substitutional solid solution alloy of pure nickel containing 1.16 pct Sn. All the materials were given a high-temperature anneal (>850°C) to produce a stable grain size of 7 to 10 grains per linear mm. The apparatus and techniques used to obtain the present results have been described elsewhere.' In this series, grain growth was observed only in the highest-purity, vacuum-cast metal. Thus we may consider that in the other materials grain-boundary migration was prevented by either preexisting voids or solute atoms. The effect of migration on the creep ductility of the above materials can be seen from Fig. 1, which

Jan 1, 1962

By E. F. Adkins, R. W. Douglas

The variation of the spectral emissivity of osmium and ruthenium with temperature can be expressed by the following relations: DURING a study of the sintering characteristics of osmium and ruthenium, discrepancies in the previously accepted melting points of the metals were noted. The melting temperatures had not been measured at the time of the work, but were estimated in the literature as 2700°C for osmium and 2450°C for ruthenium.' A recent investigation by Baird2 has shown the melting temperatures of osmium and ruthenium are 3000" and 2250° C, respectively. In the present work, osmium bars sintered at temperatures as high as 2900° C showed no evidence of melting, whereas ruthenium showed definite evidence of melting at temperatures as low as 2250°C. In view of the apparent discrepancies, the melting temperatures of both metals were determined. The spectral emissivities of both metals were determined as an aid to studies of the sintering characteristics of these metals. MATERIALS AND PROCEDURES The materials used in these studies were metal powders supplied by Englehard Industries, Inc., through the courtesy of The International Nickel Co. Analytical data from three laboratories, although not in complete agreement as to the purity of the material or the major impurity elements, indicated that the maximum impurity levels were 0.5 and 1.0 wt pct in osmium and ruthenium, respectively. The metal powders were pressed to 1/4 by 1/4 by 6-in. bars at 20Tsi using carbon tetrachloride as a lubricant. The pressed bars were presintered 1 hr at 1200°C after heating 1 hr at 400°C. The presintered densities of the several bars of the metals ranged from 65 to 80 pct of ideal density. Specimens were self-resistance heated in a vacuum sintering bell. Temperatures were measured with an L&N, disappearing filament optical pyrometer. True temperatures were read at the base of an 0.30-in.-diam, 0.150-in. deep hole drilled into the center of a presintered bar. Apparent temperatures were read from the surface of the bar adjacent to the hole. MELTING POINT DETERMINATION The melting temperature of the metals was determined as the temperature at which a slight additional increase in current through the specimen resulted in a reduced temperature at the base of the hole. The apparent reduction in temperature is a result of the liquid metal filling the hole, thus altering the black-body conditions. The melting points of osmium and ruthenium, based on three deter-

Jan 1, 1962

By J. F. Butler, H. W. Paxton

The vapor pressures of manganese in equilibrium with several alloys in the iron-manganese-carbon system between 1200° and 1275°K have been measured using the Knudsen effusion technique in conjunction with a vacuum microbalance. The effect of orifice area of the effusion cell upon the measured pressure has been determined. The binary iron-manganese system shows small negative departures from ideality, and the system of mixed carbides, (Fe, Mn)7C3, in equilibrium with graphite behaves ideally. THIS work is a continuation of the investigations in which the Knudsen effusion method has been used to determine thermodynamic activities in systems and at temperatures of interest to metallurgists. In a previous publication,' the free energy of formation of Mn7C3 was determined and some preliminary work on the solution behavior of this carbide with the hypothetical "Fe7C3" was reported. The present work deals with this latter topic and also includes data on the binary ir-on-manganese system. EXPERIMENTAL METHOD The Knudsen effusion method was used to measure the vapor pressure of manganese in both the alloy and carbide sections of this investigation. This dynamic method of vapor pressure measurement presents a problem when studying solid alloy systems in which one of the components has a much larger vapor pressure than the others. Over-all depletion of the alloy in the most volatile component will occur during evaporation so that the pressure of that component will decrease. Even more serious than the over-all concentration change is the surface depletion of volatile component in the alloy brought about by the slow rate of diffusion of this component from the interior to the surface of the solid particle. Since knowledge of this surface composition is necessary in order to relate it to the activity determined through the measurements, changes in surface composition from the analyzed bulk composition are to be avoided in dynamic vapor pressure studies of solid alloys. The system under investigation in this study presents the problem of surface depletion of manganese since its pressure at 1230°K is 105greater than iron and 1020 greater than carbon. Since the existence of a volatile manganese carbide had been ruled out previously,' the high manganese pressure relative to iron and carbon insured that the only species leaving the effusion cell was manganese. Therefore, the effusing species required no analysis so that the manganese pressure was determined directly from the weight loss of the effusion cell. In order to detect small weight losses near the beginning of effusion, a vacuum microbalance was used to weigh the cell continually. These initial weight loss data allowed the rate of manganese effusion to be determined before the surface of the alloy became depleted in manganese. The apparatus used in this investigation is shown in Fig. 1. Temperature was measured using chro-

Jan 1, 1962