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I;. D. Godshall, Everett, Wash. (communication to the Secretary) : In Mr. Morse's interesting paper several statements occur which seem to require correction and comment. This is the more appropriate, since Mr. Morse has mentioned me by name, and has cited my "Review of the Russell Process,"* so that silence on my part might be taken as indicating an assent which I cannot give. On the first page of his paper Mr. Morse says that the " goingback " of chlorination was " the only difficulty encountered at Aspen," and adds that he has " never seen any explanation " of the cause. The plain inference is that he now fills this complete

Jan 1, 1896

By Elmer W., Pehrson

NOT much serious consideration was liven to the military aspects of raw materials before World War 1. Following the outbreak of war in Europe in 1914, however. this situation was promptly changed. Disruption of allied shipping and German submarine warfare soon cut off a substantial part of the material the United Staten was accustomed to receiving from overseas. At the same time, raw material requirements rose rapidly as the tempo of industrial preparedness was stepped up in anticipation of war. By April 1917, when we entered the war, serious shortages threatened and consideralde attention was being given to our "deficcient" raw materials. The term "war mineral," began to appear after we became active combatants. But there is no evidence that "strategics" and "critical." as now used, had entered the lexicon of our raw materials experts during the last war nor were there apparently any officially recog¬nized list or definitions of what con¬stituted war materials. According to G. A. Roush in his book, `'Strategic Mineral Supplies," C. K. Leith, while serving as mineral advisor to the War Industries Board. compiled the first unofficial list of deficient minerals in 1917.

Jan 1, 1944

By Walter R. Crane

PAGE I. Apparatus and Methods.......... 406 1. The Magnetic Circuit...........406 2. Apparatus Employed in the Traction-Method...... 406 a. The Coils............409 b. The Pole-Pieces..........409 3. Methods of Testing Fields Produced by Different Pole.Pices.. ..409 c. Testing with a Search.Coil........410 d. Testing with Iron-Filings and Glass Tube.. .. .410 4. General Forma of Pole-Pieces.........411 e. Flat Poles............411 f. Conical Poles........... 411 g. Spherical Poles...........411 h. Chisel-Edged (Chamfered) Poles.......412 II. Magnetic Fields...........412 5. Methods of Testinq for Magnetic Permeability...... 421 i. The Rod-Method..........423 j. Method Employed in These Experiments......424 k. Difference in the Results of the Two Methods..... 425 l. The Traction-Method.........427 m. Effect of Loosening the Charge.......430 n Corrections...........432 6. Theory.............433 o. Effect of Varying Weight on Tractive Force..... 434 p. Effect of Varying Pole-Distance.......436 q. Effect of Varying Magnetization.......436 T. Effect of Varying Size.. .......437 a. Summary,........... 441 III. The Relative Magnetic Permeability of Various Minerals,. 443 The form and strength of magnetic fields have attracted much attention. especially in connection with the designing of dynamo-electric machinery—an art which has been revolution-

Jan 1, 1902

By AIME AIME

ANNOUNCEMENT on August 6 of the historic event of dropping an atomic bomb on Hiroshima, Japan, was more dramatic even than V-E day, since that had so long been forecast whereas the bomb production had been the best-kept secret of the war, even though at one time more than 100,000 people had been at work in connection with its production, and some two billion dollars had been spent on the project. Mining men had long been aware of an unexplained abnormal interest in uranium production, and suspected that something of the sort was on foot, while metallurgists were aware that various men of their acquaintance were engaged in some top secret research. The first announcement was soon supplemented by other official releases which told more about the research laboratories for theoretical and pilot studies, and the plants in Tennessee and Washington, but none of them made clear what the modus operandi is of these terrific bombs. Inquiry at Colum. bia University, where Dr. Dunning and his associates had succeeded in 1939 in splitting the uranium atom, and where laboratories known only as SAM have been feverishly active since the beginning of the war, was unproductive, since none of those officially connected with the project could give out anything beyond the official releases.

Jan 1, 1945

By W. Francis

Before attempting to describe the application of recently acquired knowledge to the classification of coal it will be as well to consider the objects at which a scientific classification should aim. Here one can not do better than to follow the example of Clarence Seyler,l by quoting from Huxley's "Classification of Animals:" "By the classification of any series of objects is meant the actual or ideal arrangement together of those which are like and the separation of those which are unlike, the purpose of the arrangement being to facilitate the operation of the mind in clearly conceiving and retaining in the memory the characters of the object in question. Thus there are as many classifications of any series of natural or other bodies as they have properties or relations to one another or to other things. But the statement of the characters of the class ... is something more than an arbitrary definition ... it expresses firstly, a generalization based on and constantly verified by very with experience; and, secondly, a belief arising out of that generalization—in other worda. the definition of the class is a statement of a law of correlation or coexistence . . . from which the most important conclusions are deducible." In that same sense writes John Stuart Mill, in the chapter on classification in his "Logic:" "The ends of scientific classification are best answered when the objects are formed into groups concerning which a greater number of general propositions can be made, and these properties more important, than could be made respectiug any other groups into which the same things could be distributed. The properties, therefore, according to which objects arc classified should, if possible, be those which are causes of many other properties, or, at any rate, which are sure marks of them." Now in the case of coal, the properties which have been used from time to time for classification purposes are the ultimate analysis, volatile matter, caking power, calorific power, burning properties, etc. Seyler has shown that there is a general law of correlation or coexistence between the ultimate composition and the other properties. The ultimate composition, therefore, of the natural series of bodies known as coal is the

Jan 1, 1930

By W. D. Robertson, Raymond C. Boettner

A study was made of the change in density during the first (transient) and second (linear) stages of the creep curve of polycrystalline copper as a function of 1) stress, 2) temperature, 3) plastic strain, 4) impurity and atmosphere effects, and 5) structure, including single crystals. Voids were not observed in single crystals strained 15 pct at 500°C, or in a polycrystal-line aggregate produced by recrystallizing a single crystal, within the limit of sensitivity, Ae/e = 1 x 10-4. It appears that voids are heterogeneously nucleated at grain boundaries by an insoluble phase, or phases, which can be removed by directional solidification. The principal controlling mechanism of void growth appears to be condensation of vacancies at grain boundaries. Vacancies are transported to a boundary and condense as a consequence of the tensile stress component across the boundary, which depends on the orientation and configuration of the boundary plane and on boundary shear across ledges and other irregularities. The ultimate source of vacancies is the free surface and diffusional transport is by way of the boundary plane. PREVIOUS investigations have dealt with the nucle-ation of voids at grain boundaries under creep condition~'-~ and with the connection between grain boundary voids and subsequent brittle fracture.5-7 Growth of voids during the creep process, particularly in the transient and linear stages of creep, has not been studied with the same intensity. Therefore, it seems pertinent to investigate the process of void growth with respect to the related creep curve, and the morphology of growing voids with respect to the structure.

Jan 1, 1962

By W. Rostoker

PART of a program of research on the Ti-A1 system1 involved a study of the lattice parameters of the titanium-rich a solid solution, which has a hexagonal close-packed structure. For this work, a 14 cm Debye-Scherrer powder camera and filtered CuK, radiation was used. For each pattern, the parameters were calculated by a least squares solution of the five strongest high angle lines. This provides an accuracy of i0.005A or better. The results are shown graphically in Fig. 1. It will be seen that an unusual change of slope occurs in the curve for the C parameter at high aluminum contents. Such anomalous changes in slope have been recorded by RaynorV or several magnesium-rich solid solutions. The effects were interpreted in terms of a special contribution to the lattice distortion due to factors of electronic origin predicted by Jones." Jones' theory, in substance, suggested that an unusually large expansion of the lattice would begin when the electron per atom concentration in the alloy was increased to a value at which an overlap just began from one Brillouin zone to another. Con-

Jan 1, 1953

By E. M. Wise

IT is known qualitatively that the recrystallization behavior of platinum is dependent upon the amount and particularly the nature of impurities present, the amount of prior cold-work and the annealing time and temperature, but published data are limited. A study of the effects of cold-work and annealing temperature on the hardness of a sample of very pure platinum was undertaken to supply part of this information. CONCLUSIONS 1. The platinum used in the experiments had a probable platinum content of 99.99+ per cent, and had the following mechanical properties in the completely softened condition: Vickers hardness number, 39.4; ultimate tensile strength, 19,340 lb. per sq. in.; proportional limit, very low; elongation, 37.5 per cent in 2 inches. 2. The effect of cold-rolling on the hardness is shown in Fig. 1. The hardness increases rapidly up to 10 to 15 per cent reduction and more slowly up to about 75 per cent reduction, beyond which it increases more rapidly. 3. The recrystallization temperatures for a 15-min. anneal, after cold-rolling 19, 39.5, 50.8, 66, 80.5 and 89.5 per cent reduction in thickness, are approximately 765°, 700°, 635°, 600°, 545° and 425°C., respectively. 4. The recrystallized grain size of this platinum is a function of the percentage of cold reduction, being larger the lower the percentage of cold-work. 5. Little or no grain growth resulted from subjecting recrystallized samples to higher temperatures or annealing for longer times.

Jan 1, 1940

By Carle R. Hayward

The growing importance of metallography has caused a corresponding interest in the improvement of apparatus for preparing specimens of metals and alloys for microscopic examination. The purpose of this paper is to describe an electric heating-furnace, a grinding- and polishing-machine, and a device for mounting specimens, which are used in the metallographical work at the Massachusetts Institute of Technology. These three pieces of apparatus were designed and made in the laboratory of the Institute, and each possesses some original features which may be of interest. Electric Heating-Furnace. The accurate control of heat necessary for metallographic work is best obtained by the electric-resistance furnace. Uufortunately, however, even the platinum-wound furnaces cleteriorate with use and ultimately burn out, while the cheaper resistance-materials are often short-lived. Since the resistance-coil must be replaced from time to time, it is of advantage to be able to make this change with as little trouble as possible, and this is an important feature in the furnace shown in Fig. 1. A is a cylindrical galvanized-iron can, with two handles, B. A porcelain tube, C, passes through the central hole in the cover of the can and rests upon the asbestos disk, D; the bottom of the tube is held in place by the asbestos ring, 3. The space, F, around the tube is filled with powdered magnesia. G is an ordinary assay-crucible, with the cover inverted so as to present a smooth top for supporting a second porcelain tube, H. The latter is wound with " Excello " resistance-tape, 0.014

Jan 1, 1912

By Laurance Reid

HIGH compression ratios, resulting from high injection pressures and relatively low recovery process pressures, constitute a major problem, which has confronted those engaged in gas recycling for condensate production since the beginning of that practice. Despite the numerous process developments and improvements, no entirely satisfactory solution for this prob-lem has been presented to date. Often, where the residue gas from the recovery process must be recompressed for subsurface injection, there is a substantial difference between the required injection pressure and the plant-operating pressure required to produce maximum recovery of condensate. These limitations result in high compression ratios, which, in turn, neces-sitate excessive compressor investment and operating cost. As an alternative, the operating pressure may be increased in order to lessen the compressor requirements but such a saving often is purchased at the expense of decreased condensate recovery, caused by operation at the higher pressure. Regardless of the choice, the net result is a diminished return on the capital invested in the project. The goal of future development in this field must be the complete recovery of all valuable hydrocarbon components in the reservoir fluid at pressures that, regarded as compressor suction pressure, will require minimum compressor horsepower to inject the residue gas into the formation. A com-pression ratio of 1.5 has been established as an optimum for modern compressor equipment." Therefore, in order to con-form to this optimum condition, a 3000-lb. injection pressure would require that the condensate recovery process be operated at 2000 lb. per sq. inch.

Jan 1, 1940

By P. Chaudhari, Michael B. Bever

The heat of solution at infinite dilution of selenium in bismuth, the heat of mixing of selenium and bismuth, and the limit of solubility of selenium in bis~rzuth have been determined at 573, 623; and 663°K by metal solution calorimetry. The heat of forrrzation of the compound Bi2Se at these temperatures has been determined from the heat effects associated with the precipitation of the compound from a saturated solution oj selenium and bismuth. The published information on the thermodynamic properties of the system Bi-Se is limited. The heat of solution at infinite dilution of selenium in bismuth at 623°K has been measured.' The heat of formation at 273 K1 and room temperature2 and the heat capacity at 80 K3 of the compound Bi2Se3 have been reported. An estimate of the heat of formation of the compound BiSe at room temperature has been published.2 Information on the phase relations in the system Bi-Se is available.' In the investigation reported here the following quantities have been determined at 573", 623", and 663°K: 1) the heat of solution at infinite dilution of selenium in bismuth, 2) the heat of mixing of selenium and bismuth in bismuth-rich solutions, 3) the limit of solubility of selenium in bismuth, and 4) the heat of formation of the compound BizSe. These quantities were determined by the addition of selenium to bismuth-rich solutions in a metal solution calorimeter. The determination of the heat of formation at the tem- perature of the calorimeter bath involved the precipitation of the compound from a saturated solution in the calorimeter. 5,6 This method differs from that commonly used which requires the addition of the compound and of a mechanical mixture of its components and yields the heat of formation at the temperature from which the additions are made (273 K EXPERIMENTAL PROCEDURE AND CALCULATIONS The solution calorimeter has been described in detail.' Pure bismuth (99.999+ pct) was used as the bath at the start of a run. The calorimeter was calibrated with small amounts of bismuth added from 273°K; the differences of the heat contents of bismuth at 273°K and the temperatures of the baths are listed in Table I. After the calibration, additions of hexagonal selenium (99.999+ pct) were made. Loss of selenium by evaporation was negligible. No unusual experimental difficulties were encountered.9 The differences in the heat contents10 of selenium at 273°K and the temperature of the bath, listed in Table I, were subtracted from the measured heat effects to give the "adjusted heat effects". The methods by which the heat of solution at infinite dilution, the

Jan 1, 1968

By C. R. Sandberg, L. S. Gournay, R. F. Sippel

The effect of fluid-flow rate and fluid viscosity on oil-water relative permeability determinations was studied using the "dynamic flow technique." In this work relative per-nleability curves were obtained for homogeneous small core .samples from several sandstorle outcrop form-utions. Radio-tracers were used for the determination of fluid saturation and for the detection of saturation gradients. Cobalt-60 in the form of cobaltous chloride was used as a water-phase tracer in some of the experiments. Iodine-131 in the form of iodobenzene and Mercury-20-3 in the form of mercury diphenyl were used as oil-phase tracers in other experiments. Flow rates for each phase were varied within a range of 2.5 to 140.6 ml/hr. Oil-phase vis-cosities under flowing condition,> were varied from 0.398 to 1.683 cp. The relative permbilities ob-tained were found to he solely a function of saturation and independent of flow rare, provided there was no .Saturation gradient induced in the core sample by "boundary effect." Even though equilibrium with re-sped to flowing conditions was obtained at the lower flow rates, where a saturation gradient exists, this equilibrium is of a "contingent"-type rather than the "steady-state" equi-librium implicit in the relative per-meability concept. The only effect of increasing the oil or non-wetting phase viscosity was to decrease the flow rate required for the elimina-tion of the boundary effect. Fairly good agreement between experimentally determined and calculated values of the boundary effect was obtained when the non-wet-ring oil phase was the only Flowing phase. INTRODUCTION In the characterization of reservoir rock, as well as in the solution of reservoir production problems, it is most desirable to have reliablc rela-tive permeability measurements for the rock and fluids of interest. Many techniques have been developed for the laboratory determination of the relative permeability of both large and small core samples. In varying degree, difficulties attend the use of all of the methods. Each of the methods requires the metered flow of fluids of known viscosity through the core sample under conditions wherein the pressure drop in the individual flowing phases can be measured or closely approximated. Since the relative permeability is a function of the saturation and distribution of the flowing fluids, some means of obtaining such information is also required. The laboratory determination of the relative permeability of a sample should give the same relative permeability saturation relationship that would exist if the sample were in place in the oil reservoir. The attainment of this objective is complicated by the fact that the use of small core samples for laboratory measurements is usually necessary. As a result, errors in measuring the relative permeability arise from boundary effects at either the fluid input or output ends of the sample; no significant boundary effect is anticipated at the sides of the sample normal to direction of fluid flow. At the input end of the sample a boundary effect exists if the flow fluids are not com- mingled as they would be in the reservoir. At the output end of the sample a boundary effect exists as a result of discontinuity of the capillary properties of the system. Here the flowing fluids leave the small flow channels and enter a collecting system having much enlarged flow channels. Thus, there is a tendency for the wetting phase to be retained by the core sample because of the attraction of the core sample for the wetting fluid. No reference is made to these boundary effects in either Darcy's equation or in the relative permeability concept. As a consequence the saturation effect peculiar to the input end of the core sample may cause an error in the effective permeability measurement, since some portion of the core sample must be utilized for commingling of the flow fluids. At the output portion of the core sample a saturation gradient or a saturation change along the axis of flow results. Since relative permeability is a function of fluid saturation, this saturation gradient may cause a variable permeability measurement, especially since extent and character of the saturation gradient can vary with fluid-flow rate. The most convenient method of minimizing the boundary effect, especially at the output end of the sample, is to flow the fluids of interest through the core sample at such high rates that the capillary forces arc insignificant as compared to the viscous forces involved in the fluid flow. Since recent work of a preliminary nature has indicated that fluid dispersion in the porous medium increases with the flow rate, the high flow minimizes the boundary effect at the input end of the core sample by enhancing the mixing of the fluids.

By M. E. Straumanis, J. -P. Krumme

In basic ([KOH + KCl] with a total polarity of 2) or acidic (2N H2SO4) electrolytes and at anodic current densities of more thun 2 to 4 ma per sq cnz, n-type GaAs single crystals of lozo resistivity preferentially dissol~je forming etch tunnels with triangular or civc~ilay cross sections and of a width between 0.5 arid 5 p. These etch tunnels are oriented along any one of the four possible (111) directions of GaAs. However, their growth occurs only in one direction of a given (111) whick apparently is determined by the atomic sequence Ga —As (and not the rezlerse) in respect to an individual valence bridge in the crystal. It is concluded from comparison with the cubic lattice structure of GaAs that the etch tunnels represent macroscopic evidence for the tetrahedral bonds and their polar properties. If the anodic current density is increased the tunnel fomation results in the development of a fibrous surface layer consisting of GaAs. The latter separates frorn the substrate (in an anodic s~irface disintegration process) by the growth pressure of an As,0, filnz forming in the interior of the fibrous layer, 100 to 200 µ under the surface, at more than about 50 ma per sq cni. The fibrous GaAs film has the same crystallographic orientation as the substvate and represents a skeleton of the original crystal. Since the etch-tunnel density in a separated GaAs layer is about 108 c?n-', and the etch tunnels develop only along (111) in a given polar direction, it is assurraed tlmt the dislocations have no influence on the growth of these tunnels. ElECTROLYTIC treatment of smooth surfaces of poly- and single-crystalline GaAs at high anodic current densities causes the formation of porous surface layers.' This phenomenon suggests comparison with effects being observed with magnesium,' indium,, gallium,4 and aluminum5 and known as "anodic disintegration". The purpose of the present paper is to explore and to explain the reasons for the formation of such surface layers on GaAs and, in particular, to investigate the influence of the lattice polarity of this III-V compound semiconductor in the (111) direction on the anodic dissolution behavior. GaAs SINGLE CRYSTALS For the experiments described below GaAs single crystals from the Monsanto Co., St. Louis, Mo., were used. Their impurity levels were below 1 ppm and their dopant levels between 1 and 100 ppm. They were grown in (111) using the Czochralski or the gradient-freeze technique. The crystals had n-type conductivity and electric resistivities between 1 and 5 ohm-cm. EXPERIMENTAL The GaAs single-crystal rods were cut perpendicularly to (111) into wafers of about 1 mm thickness using a wire-blade crystal slicer and an aqueous slurry of Sic or a diamond saw. The orientation of the faces of these wafers were checked by Laue back-reflection patterns. If there was a deviation from (111) the faces were abraded under a certain angle using grinding paper and distilled water. The damaged surface layer was removed from each crystal by chemical etching with a mixture of 1HF:1HNO3: 1H20 or 2HF:1HNO3:2HAc (glacial). {110) faces were obtained by mechanical cleavage, producing surfaces which did not require a further treatment. The GaAs wafers were mounted using "alligator" clamps instead of soldered electrical contacts.' Only the bare crystal surfaces were dipped into the electrolyte. The clamps were coated with insulating wax to prevent any contact with the electrolyte. The experiments were carried out in aqueous 2 N H2so4,' or in an aqueous solution of KOH and KCl1 (1 mole KOH + 1 mole KCl in 1000 cu cm solution). Anodic current densities up to several hundred ma per sq cm were applied for periods between 30 sec and 2 hr. For the purpose of investigating the initial steps of disintegration the anodic current density applied never exceeded 20 ma per sq cm. The films which partially separated from the anodic surfaces under high-field conditions were treated with KOH to further their detachment by dissolving the As2O3 formed. The washed and dried films were pasted to strips of filter paper, and Laue pictures were made. The back-reflection patterns obtained were compared with those of the original anode surface before and after anodic dissolution. Furthermore, space reciprocal lattices7 were constructed from asymmetric rotation crystal patternsa which permitted the determination of the crystallographic orientation of the detached films of the corrugated anodic surfaces. The disintegration products were identified from assymmetric powder patterns.8 The polarity of the {111) faces was determined by chemical etching with mixtures of 1HF:1H2O2(30 pct): 2H2O or 1HNO3:2H2O. Different patterns on each of two inverse (111) sides appeared.'-l8 The correlation of these patterns to the Ga{111) or the As(111) side has already been established by the use of light figures,18-20 by X-ray diffraction near the absorption edges of gallium and arsenic,'lmZ4 and by LEED measurements.25 The geometric structure of these surfaces and the interior of the anodically attacked crystals were observed and photographed with a high-power microscope using oil immersion objectives up to magnification of X1720.

Jan 1, 1968

The total estimated production of coal in the United States during the first century and a quarter of mining is shown in Table 20. This is the total of the production of the various states already shown in the various tables, and is believed to be the first statement of this sort made. No such table prepared from limited data can be accurate, but it is the writer's opinion that the totals shown are less than those actually produced. It was thought that this study would enable a reasonably accurate account of the movement of coal down the Ohio and Mississippi Rivers to be written. The searches made have shown that at this time the data do not exist from which such a study can be made, but some of the facts collected may be useful to future students.

Jan 1, 1942

By A. Raman, P. P. Singh

The constitution of the La-Rh system was studied by powder X-ray diffraction, metallopaphic, and differential thermal analysis techniques and an equilibrium diagram is presented. Eleven intermediate phases occur in the system and the crystal structural data for nine of them were determined. La3Rh crystallizes in an orthorhombic structure of undetermined type, whose unit cell is obtained by doubling the 'a; and 'c,,' edges of an FesC type unit cell. The other intermediate phases of the system are LarRh-3( undetermined structures also occur in the system. LaRh, undergoes a polymorphic phase transformation at 1240°C. LaRh3 and La2Rh7 also exhibit polymorphisnz. The phases Laah and LazRh7 melt congruently. The latter undergoes a eutectoid transformation into LaRh, and Rh at 1205°C. Laah3 is formed by a peritectoid reaction between Laah and La,Rh,,. The other Phases result from peritectic reactions between the liquid and the adjacent rhodium-rich phases. The intermediate Phases of the La-Rh system are compared with those of the La-Co and La-Ni systems. DURING the course of a detailed investigation to study the occurrence of CrB, FeB, A1B2, and related structures in the rare earth alloys it was found that much information is lacking for the rare earth noble metal systems. Although the structures of several rare earth alloys containing the noble metals at the AB and AB2 stoichiometries have been reported, the occurrence of related structures at other stoichiometries has not been studied. We have initiated a project to study the crystal structural features of selected rare earth-rhodium alloys and to map the equilibrium diagrams of representative systems with conventional methods. The results of our investigation in the La-Rh system are presented in this paper. Two phases were known in the La-Rh system. LaRh has the CrB-type structure.' LaRhz is a MgCu2-type Laves phase.z EXPERIMENTAL PROCEDURE Alloys weighing less than 1 g were prepared from commercially pure lanthanum (99.9 pct +), supplied by Lunex Company, Pleasant Valley, Iowa, and rhodium (99.92 pct +), supplied by Engelhardt Industries, Newark, N.J., in a conventional arc melting furnace under argon atmosphere. The buttons were turned upside down and remelted three times to insure homogeneity in the samples. Since negligible loss of material was encountered during melting, a chemical analysis of the alloy buttons was not undertaken. Powder specimens for X-ray diffraction studies in the as cast state were then prepared. The buttons were wrapped in thin molybdenum foils and homogenized by heating in vacuum at suitable high temperatures for more than 1 week. They were then broken into three or four pieces for annealing experiments. The pieces were wrapped in molybdenum foils and annealed at various temperatures in evacuated quartz capsules. The annealing was carried out for 2 hr at or above 1200°C, 1 day at temperatures close to llOO°C, 2 days at 1000°C, and for 1 week at temperatures below 1000°C. After annealing the alloy pieces were again broken and powder specimens for X-ray diffraction were prepared. The powders of the lanthanum rich alloys with more than 80 at. pct La were prepared by filing. The filings were sealed in molybdenum tubings and stress-relieved at 600°C in vacuum. It was not deemed necessary to stress-relieve the powders of the other alloys, since the alloys were very brittle and were ground easily. POWDER X-RAY DIFFRACTION X-ray diffraction photographs of powders (-325 mesh size) of the alloys in the as cast and annealed states were prepared in a Guinier-de Wolff focussing camera with copper K, X radiations. These patterns were studied to identify the stoichiometries and the crystal structures of the intermediate phases. The lattice parameters of the phases were calculated after minimizing the differences between the observed sin2 6 values, calculated from the diffraction angles 8, and the sin2 8 values, calculated using approximate lattice constants obtained from a few lines. These differences were minimized manually to less than 0.0005. The latLice constants are judged to be accurate to *0.005A for values less thp about 10A and to k0.01~ for values greater than 10A. The relative intensities of the lines were calculated using a computer program written by Jeitschko and Parthk.~ No attempt was made to refine the atomic positional parameters in the phases. METALLOGRAPHY The phase equilibria in the investigated alloys in the as cast and annealed states were also studied by metallographic examination. The polished specimen surfaces were etched with 10 pct picric acid in alcohol (alloys up to 25 pct Rh), concentrated picric acid (from 25 to 37.5 pct Rh), 2 pct nital (40 to 50 pct Rh), 10 pct nital (from 50 to 66.7 pct Rh) and with concentrated 48 pct HF for the other rhodium-rich alloys. Selected microstruture~ were then photographed using a Po-laroid Land camera. THERMAL ANALYSIS Differential thermal analysis of the alloys was carried out in DTA-668 Stone differential thermal ana-

Jan 1, 1970

By H. Foster Bain

Jan 1, 1910

By Paul Rhedey

Various commercial pelroleum cokes were heat-1,reated at temperatures between 500° and 1500°C, in a nitrogen atmosphere, in laboratovy induction furnaces. The rate of tenlperature rise was varied betzveen 10" and 300°C per min, or the green cokes were flash-calcined, orv a combination of heating rates was used. Changes in the rate of heating had only negligible effects on the degree of' calcination as characterized by mean crystallite thickness and the chemical properties of the calcined coke. The physical structure of the cake was however significantly affected when rate of heating during calcination exceeded 50°C per min over the temperature range of 600° to 900°C. Surface-accessible porosily increased with the .rate of temperature rise, and this was accompanied by a change in pore size distribution. Source and properties of the green coke also had an influence on the structure of the calcined coke. The evidence presented suggests a similar mechanism of porosity development in petroleuiiz coke during calcination in industvial equiplnenl, such as rotary kilns. An increase in surface accessible povosity incveased the pitch binder requirement when the coke was used as aggregate in Soderberg paste. A correlation was established between calcined coke porosity and paste binder requiremenl. ManY results have been published on the changes of properties of petroleum coke during calcination, such as chemical composition, real density, electrical resistivity, crystallite and pore structure. The correlation of these properties with temperature of calcination and time at maximum temperature has been rather well established in both laboratory and pilot plant experiments. Surprisingly little attention has been given however to the effect of calcination conditions, such as rate of temperature rise or furnace atmosphere, on the chemical and structural properties of the calcined coke. It has been observed that petroleum coke, when calcined in industrial equipment, acquires higher porosity and lower real density than those attainable in laboratory furnaces at apparently identical calcina- tion temperature and soaking time. This paper describes a study of the effect of rate of heating during calcination on calcined coke properties using green petroleum cokes of different volatile matter, hydrogen, and sulfur content. An attempt was made to correlate the changes in coke structure with the flowability of anode paste of the type normally used in aluminum reduction cells. EXPERIMENTAL Petroleum Cokes Used. In the study of release of volatile matter and sulfur during calcination and the effect of rate of heating on calcined coke properties two delayed cokes of different sulfur contents were used. The results of analysis of the green cokes are given in Table I. In the study of the effect of flash calcination thirty-six commercial petroleum cokes from twelve different refineries were used with a range of properties shown in Table 11. Calcination Conditions. Calcination experiments were carried out in a laboratory induction furnace. In each run a 200-g sample of dry green coke sized to 10 by 65 Tyler mesh was calcined in a graphite crucible. The crucible containing the sample was placed in the middle of a stack of eight others filled with metallurgical coke to reduce temperature gradients within the sample. Temperature was measured by two Pt, Pt-10 pct Rh thermocouples and controlled by a Celectray instrument. The two couples generally agreed within 5°C. In the study of volatile matter and sulfur release the samples were heated to temperatures in the range of 500" to 1500°C at a rate of 10°C per min in a nitrogen atmosphere and held at the final temperatures for 30 min. In the study of the effect of heating rate on calcined coke properties the desired rates between 10' and 300°C per min were obtained by manually adjusting the power input. Flash calcination was carried out by dropping 100 g of the green coke into the graphite dish preheated to the calcination temperature. Because of the small heat capacity of the furnace the coke was introduced in 20-g portions at a time. For this purpose a 2-in.-long nipple between two 1-in. gate valves installed on the top flange of the furnace served to provide a gas seal while feeding coke to the furnace. It was estimated that the temperature of the coke reached that of the furnace at a rate of approximately 1000°C per min. Holding time at final temperature was also 30 min. Calcined Coke Proper- Determined. Porosity was determined on 20 by 35 Tyler mesh samples using an Aminco-Winslow mercury pressure porosimeter with an operating range of 1.8 to 3000 psi absolute pressure (100 to 0.05 p pore diameter range).' Apparent density was obtained by the mercury poro-simeter. It represents a particle density of the 20 by

Jan 1, 1968

[FUQUA, H. B. and Thompson, B. E.: Oil and Gas Development and Production in North Texas for 1933, 107, 320; for 1934, 114, 417 Oil and Gas Development in West Texas 114, 438 FURMAN, W. F.: Heat and Corrosion-resisting Alloys. Printed in Oil & Gas Jnl., June 13, 1935 Furnace-bottom sand, uniformity, 73, 390 Furnace control, Isley apparatus, M27, 502 Furnaces (See also Holt-Dern; Blast Furnaces; Roasters; Wirebar, etc.): annealing: electric, 89, 424 gas-fired, 89, 425 gas vs. wood for nonferrous metals, 89, 422]

Jan 1, 1936

By J. R. Bell, W. J. Childs, J. H. Bucher, G. A. Wilber

A technique for determining recrystallization times as short as 0.10 sec was developed utilizing the "Gleeble", a commercially available testing system designed for the study of short-time, high-temperaLure themal and mechanical processes. The procedure consisted of heating a small tensile specimen to a given temperature of hot deformation, loading to a given reduction in area, unloading, delaying various intervals at temperature, and then reloading- to failure. The magnitude of the ultimate load obtained upon reloading decreased with delay lime as recrys-lallization proceeded. The technique was applied to austenite recrystallization in AISI 1010 and AISI 1010 uith 0.02 pct Cb steels. For each steel the reduction in area given the specimen on the first pull was mainlairred at 30 ± 5 pct and recrystallization times deterntined at various temperatures. The results indicaled a significantly slower rate of recrystallization for the columbium-modified composition, suggested the presence of- a recovery stage in the softening process , and indicated a greatly increased softening rate at a temperatuve where significant allotropic transformation to a partially ferritic Structure could occur. In recent years increasing attention has been paid to the fact that the process of recrystallization of austenite deformed at elevated temperatures is far from instantaneous at many practical hot-working temperatures.1-3 This realization has given rise to such terms as hot cold-working1 or warm-working,2 These terms generally describe processes where the recrystallization rate at the temperature of deformation is slow enough to have an appreciable effect on mechanical properties despite a relatively high deformation ternperature. The mechanical properties of interest can be either the properties at the deformation temperature as in hot-workability studies4 or the room-temperature properties after cooling as in the many recent studies of various thermomechanical processes172 where heat treatment and deformation are intentionally combined to give a unique set of room-temperature properties. Because of this interest in processes where the austenite recrystallization kinetics can be an important variable, the development of quantitative methods of following the course of short-time, high-temperature recrystallization has received increasing attention.l,3,5 The experimental methods to date have, in general, relied upon rapidly deforming the austenite, holding at temperature for various brief intervals, quenching as G.A.WILBER and W. J. CHILDS, Members AIME,are Research-Fellow and Professor, respectively, Rensselaer Polytechnic Institute, Troy, N. Y. J. R. BELL and J. H. BUCHER, Member AIME, are Research Engineer and Research Supervisor, respectively, Graham Research Laboratory, Jones & Laughlin Steel Co., Pittsburgh, Pa. Manuscript submitted March 13, 1968. IMD. rapidly as possible, and then using room-temperature measurements to follow the recrystallization process. Although such methods can be successfully applied to certain alloy steels, the existence of the allotropic transformation during cooling of plain-carbon or low-alloy steels tends to obscure the results. Thus, such room-temperature measurements as hardness and X-ray line widths do not correlate well with the extent of austenite recrystallization before quenching,5 and results based on room-temperature microstruc-tural observations are dependent upon the success in correlating the observed structure with the prior aus-tenitic grain structure.1,3,5 The purpose of the present work was to develop a quantitative method for the determination of short-time, high-temperature recrystallization rates, based on measurements made at the temperature of deformation. EXPERIMENTAL TECHNIQUE The basic technique consisted of heating a small tensile specimen to a given temperature of hot deformation, loading to a given reduction in area, unloading, delaying various intervals at temperature, and then reloading to failure. The data were obtained in the form of traces of load and elongation as a function of time. Due to the high deformation temperature, the strain hardening introduced during initial loading was progressively annealed out with holding time after unloading and the loads obtained upon reloading decreased as this softening proceeded. Although the value of the second load at any Consistent point On the load-elongation curve could have been used as a measure of the degree of softening, the most convenient to use was the ultimate load. The softening indicated by the decrease in the second ultimate load with time is essentially a process of annealing of cold-worked material at a high deformation temperature. Although some recovery grain growth may contribute to such a softening process, it is generally considered that the major softening which must take place to achieve complete removal of substantial Strain hardening will occur by the formation of new, stress-free grains. As the results of this work indicate that essentially complete removal of strain hardening did in fact occur. the primary softening process will be attributed to recrystallization, and specific reference made where it appears that other mechanisms may be contributing to the total observed softening. It would, of course, be of interest to attempt to correlate the results of this work with the actual austenite fraction recrystallized as determined by other techniques. This was not attempted in the present work because it would have required running a large number of additional specimens and, as discussed previously, there is limited assurance that the results would accurately reflect the prior austenite fraction recrys-

Jan 1, 1969

By Charles Behre

THIS paper deals with recent geologic studies in the slate belt of Northampton, Lehigh and Berks counties, Pennsylvania. The work was conducted under the auspices of the Pennsylvania Topographic and Geologic Survey. Three years have now been spent in detailed consideration of the economic geology of this region. In the field, particular attention was paid to the bearing of geology on quarry development and property valuation and the object of this paper is to summarize the results from that viewpoint. Excellent studies of a somewhat similar nature have already been carried out by Bowles,1 but with the emphasis upon the details of quarrying and fabricating methods, rather than upon the geologic relations. THE NORTHAMPTON-LEHIGH-BERKS DISTRICT Location The region here discussed lies in east-central Pennsylvania and extends southwestward from Delaware River, on the New Jersey line, to the Schuylkill in north-central Berks County. It is an elongated belt occupying the northern sections of the three counties mentioned and lying along the southern edge of Blue Mountain. Its length is about 50 miles and its average width five or six, though in places it attains a maximum of 10 miles.

Jan 1, 1928