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Coal Division Industrial Minerals Division Minerals Beneficiation Division Mining, Geology and Geophysics Division Council Will Mitchell, Jr, Chairman (MBD), Kenneth L Cook, Vice-Chairman (MGGD). Edward L Clark (MGGD), Raymond B Ladoo (Ind Min Div), Sandford S Cole (Ind Mm Div), Norman L Weiss (MBD), C T Hayden (Coal), H F Yancey (Coal), Clayton G Ball (MED), P De Bruyn (MIED), Arnold Buzzalini, Secretary, AIME, 29 West 39th Street, New York 18, N Y Mining Branch Advisory Committee Will Mitchell, Jr, Chairman, Grover J Holt, J B Morrow, J L Gillson, Edward G Fox, S S Cole, Roger V Pierce, Norman L Weiss. H C Weed. J R Van Pelt

Jan 1, 1956

By Robert W. Hendricks, John B. Newkirk

A simple method is described for determining the orientation of a single crystal by means of a cylindr cal X-ray camera. Orientation setting to within ±1 deg is attainable by a stereographic analysis of a single cylindrical Laue pattern produced by the originally randomly mounted crystal. Final precision adjustments which permit orientation of the crystal to within ±5 min of arc from the desired position can be made by the method of Weisz and Cole. A chart, originally Presented by Schiebold and schneider7 and which allows a direct reading of the two stereographic polar coordinates of the corresponding pole of a given Laue spot, has been recomputed to aid in the stereographic interpretation of the cylindrical Laue X-ray photograph. Detailed instructions for the use of the chart, a simple example, and a comparison with the conventional flat-film Laue Methods, are presented. 1 HE problem of determining the orientation of the unit cell of a single crystal relative to a set of fixed external reference coordinates is fundamental to most problems of X-ray crystallography and to many experimental studies of the structure-sensitive physical properties of crystalline materials. Several techniques for measuring these orientation relations have been developed which correlate optically observable, orientation-dependent physical properties to the unit cell. Examples of such procedures include the observation of cleavage faces or birefringence, as discussed by bunn,1 or the examination of preferentially formed etch-pits, as discussed by barrett.2 Each of these methods is limited, for various reasons, to an orientation accuracy of approximately ±1 deg—a serious limitation in some experimental studies. Several other limitations decrease the generality of these methods. Of these, perhaps most notable is the absence in many crystals of the physical property necessary for the orientation technique. The most widely used methods for determining crystal orientation are variations of the Laue X-ray diffraction method. Because of the indeterminacy of the X-ray wavelength diffracted to a given spot, the interpretation of Laue photographs is now limited almost exclusively to the procedure of using a chart to determine the angular coordinates of the corresponding pole for each spot. For the flat-film geometries, either a leonhardt3 or a Dunn-Martin4 chart is used in interpreting transmission patterns, whereas a greninger5 chart is used for interpreting back-reflection patterns. A less common method of interpreting flat-film transmission Laue photographs is by comparing the Laue pattern with the Majima and Togino standards,6 or with the revised standards prepared by Dunn and Martin.4 Although this last method is applicable only to crystals with cubic symmetry, it can be very rapid and just as accurate as the graphical methods. The primary limitation of all the X-ray methods mentioned is the relatively small number of Laue spots and zones which are recorded on the flat film. Often, few, if any, major poles appear, thus making interpretation tedious and sometimes uncertain. The use of a cylindrical film eliminates this problem. Schiebold and schneider7 prepared a chart by which the orientation of the specimen crystal could be determined from a cylindrical Laue photograph. However, it was only drawn in 5-deg intervals of each of the two angular variables used to identify the Laue spots, thus limiting the accuracy of orientation to about ±3 deg. An examination of this chart indicated that if it were drawn in 2-deg intervals, crystal orientations to ±1 deg would be attainable. Subsequent use of the replotted chart has confirmed this accuracy. It is the purpose of this paper to describe the redevelopment and use of this chart, and to point out its advantages and limitations. I) CAMERA GEOMETRY AND CHART CALCULATIONS The geometry of the cylindrical camera with a related reference sphere is shown in Fig. 1. The X-ray beam BB&apos; pierces the film at the back-reflection hole B, strikes the crystal at 0, and the transmitted beam leaves the camera at the transmission hole T. One of the diffracted X-rays intersects the film at a Laue spot L. The normal OP to the diffracting plane bisects the angle BOL between the incident and diffracted X-ray beams. The point P on the reference sphere can be located uniquely by the two orthogonal motions 6 and 8 on the two great circles ENWS and BPQT respectively. Because the Bragg angle 8 (= 90 - < BOP) is always less than 90 deg, P always remains in the hemisphere BENWS. Therefore, if every possible pole P is to be recorded on the same stereographic projection, it is necessary that the projection reference point be at T with the projection plane tangent to the sphere at B.* The great

Jan 1, 1963

By N. Nakanishi, C. M. Wayman

The effect of small copper additions on the mar-tensitic transformation behavior in Au-47.5 at. pct Cd was studied by measuring electrical resistivity as a function of temperature. The transformation behavior was found to change and transformation start (M,) temperatures for both the ß to ß&apos; and ß to ß&apos; transformations were depressed substantially by the addition of small amounts of copper. Both M, temperatures were lowered approximately 70°C per at. pct Cu. Copper also had the effect of narrowing the transformation hysteresis region (resistivity us temperature), and for the alloy Au-47.5 Cd-1.5 Cu there was little or no hysteresis; in this alloy, the reverse transfmmation upon heating apparently occurs below the thermodynamic equilibrium temperature, To. THE ß phase in the Au-Cd system occurs at the electron/atom ratio 3/2, and is similar to other ß phases in alloys based on copper, silver, or gold. It is of the CsCl type, in which a considerable degree of long-range order persists to the melting temperature.&apos; The phase boundaries of the ß phase are not known precisely below 300° C, but at room tem- perature the phase exists from approximately 46 to 52* at. pct Cd.2 At low temperatures, the ß phase transforms in a diffusionless (martensitic) manner. Alloys having a composition near 47.5 pct Cd transform upon slow cooling to an orthorhombic3 phase, ß&apos;, at - 60°C. Alloys having a composition near 49.0 pct Cd, transform at - 30°C into a phase, ß", which has been recently identified as trigonal.4 Alloys having compositions near 48.5 pct Cd will transform into both the 0&apos; and 0" phases over a range of temperatures. The progress of transformations can be observed

Jan 1, 1963

By A. M. Johnson, M. M. Singh

The mechanism of failure under a drill bit is still improperly understood in spite of several investigations of the subject. Generally, the cratering process under static loading conditions is considered to be similar to that achieved dynamically by impact. This paper attempts to indicate that, although the sequence of fracturing in the two cases appear to be identical, at least some dissimilarities exist. For example, the width-to-depth ratios of the craters vary to some extent, and the amount of energy consumed per unit of volume of craters is unequal for the two different loading conditions. Prevalent rock penetration processes are dominated by methods utilizing mechanical attack on rock. It is, therefore, generally accepted that a better comprehension of the mechanism of rock failure under a wedge would prove beneficial towards improving present drilling techniques. Several attempts have been made in recent years to explain how craters are formed under a drill bit, but the mechanism of failure beneath a bit is still improperly understood. 1-11 Most investigators, to date, have inferred the sequence of events occurring during crater formation from analyses of force-time diagrams,1"6 from theoretical considerations,7 or from a study of the configurations of final craters.8-l0 These analyses have led to the presentation of widely divergent models for rock failure beneath a drill bit, ranging from brittle to viscoelastic. The cratering process under dynamic loading commonly is regarded as being similar to that obtained under gradually applied, or &apos;static&apos;, loads. But the effect of rate of loading on the action of a bit is still disputed. Some investigators11-12 maintain that there should be no such effects, whereas others have demonstrated experimentally that these exist.13-17&apos; The purpose of the investigation reported in this paper was to examine petrographically the damage done to rock under the action of a chisel-shaped wedge, both with &apos;static&apos; and dynamic loading, and to determine if rate-of-loading effects could be detected. Significant quantitative differences in crater volumes and depths were found to exist for a given consumption of energy. On the basis of this data, an attempt was made to indicate some of the rheological properties that a proposed model should possess. All the work reported herein was conducted at atmospheric pressures. EXPERIMENTAL APPARATUS AND PROCEDURE Two types of rocks were employed for most of the experiments reported in this paper, viz. Bedford (Indiana) limestone and Vermont marble. The mechanical properties of these rocks are given in Appendix A. Actually two types of Vermont marble were used, but since no marked difference could be discerned between the two varieties (as seen in Fig. 10) the data was used collectively for the analysis. Stronger rocks were not employed owing to difficulty in generation of observable craters without damage to the equipment. Six-in. diam cores were drilled from the rock samples and embedded in 8-in, diam steel pipe with 3/8-in. wall thickness, using hydrostone to fill the annulus between the core and the pipe. This procedure was adopted to confine the rock specimen so that fractures would not propagate to the edges of the cores. This goal was achieved satisfactorily for these tests because no cracks were observed to extend into the medium surrounding the rock, even when craters were formed only 1 in. from the rock core periphery. Three to four craters were formed on a core face, because the rock damage from any one crater generally did not appear to extend into the others. Whenever, interference between damaged areas around adjacent craters was suspected, the data was rejected for purposes of the analysis. The limestone and marble samples were tested with a 60-degree, wedge-shaped bit, 1 5/8-in. in length, made of tool steel. The bit shank had two SR-4 type electrical resistance strain gages, mounted axially, to record the force-time history during the loading operation. The static indentation tests were conducted using a 50-ton capacity press fitted with an adapter for drill bit attachment. See Fig. 1. The force exerted by the bit at any instant was measured with strain gages affixed to the bit shank. An aluminum cantilever, with two SR-4 strain gages mounted near its clamped end, was employed to measure bit displacement. Both sets of gages were included in Wheatstone bridge circuits,

Jan 1, 1968

By J. H. Richards, G. Derge, W. Peifer

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,&apos; and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By G. Derge, W. Peifer, J. H. Richards

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,&apos; and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By W. D. Donnelly, M. L. Rudee

THE crystallography and morphology of ?-Al3Fe precipitates in an A1 + 0.5 wt pct Fe alloy have been studied by transmission electron microscopy. The alloy was cast in cylindrical ingots, 15 cm in diameter and 60 cm in length, and cooled slowly. The measured composition was 0.527 wt pct Fe, 0.001 wt pct Mg, and 0.003 wt pct Cu. Spectrographic analysis revealed no additional trace impurities. Thin slices were cut from the ingot and reduced by more than 95 pct by rolling to a thickness of 0.1 mm with no intermediate annealing treatments. These thin sheets were then vacuum-annealed for 1 hr at 612°C and air-cooled in their capsules. Thin foils for examination in the electron microscope were prepared by electropolishing. The precipitate is found in the form of oval platelets on the (110) planes of the matrix. The major axes of the platelets are parallel to the (110) directions of the matrix, and vary in length from 1/2 to 2 p. The thickness is about 1/10 µ. Examples of platelets, both in the plane of the foil and normal to the foil, are shown in Figs. l(a) and l(b), respectively. lack&apos; found that ?-A13Fe (more correctly Al13Fe4) belongs to the monoclinic system. Using Black&apos;s structural data and simultaneous electron-diffraction patterns from the matrix and precipitates, the habit planes and directions were determined to be: (001)? 1 (110)Al [100]?|| H [001]Al The orthogonal crystallographic axes of the precipitates are accurately in the habit plane, while the measured coincidences of the directions are only within 10 deg. The major axis of the platelet is parallel to [010] in the 0. This orientation corresponds to the direction of nearest registry of the lattices.

Jan 1, 1964

By David C. Grant, Erich W. Tiepel

In situ mining is a process for recovering uranium from relatively small or low grade ore bodies. The process involves passing a lixiviant and oxidant, typically NH4HC03 and H202, through a uraniumcontaining ore body. As the solution progresses through the ore body, the uranium is oxidized from the plus four to the soluble plus six state. The bicarbonate complexed uranium laden solution is removed from the ore body and the uranium recovered in an above-ground processing plant. During the leach process lixiviant cations may be sorbed on the ore host, if the host contains exchangeable clay minerals. This report examines the implications of this clay interaction on ground-water quality, the various available in situ mining restoration methods, laboratory procedures for simulation and development of those methods, and the results of using the restoration methods in the field. Various restoration methods, including ground-water sweeping, clean water recycle, and chemical restoration are presented and discussed. The use of ore characterization, agitation leach tests, and column tests to study cation sorption and desorption, and thus, to identify and evaluate restoration methods is discussed. Ore characteristics identify the clay type and clay content, which allows the estimation of the magnitude of the cation sorption by that ore. The chemical effects of clay exchange and of chemical restoration can be examined using agitation leach experiments and packed ore column tests which also provide information on the physical effects. The agitation leach test is a relatively rapid means of determining the sorption and desorption characteristics of an ore. Unlike agitation leach tests, column tests can be used to assess the influence of solutions on permeability, on precipitation problems, and on other chemical changes. The effectiveness of using restoration methods, which were developed and tested in the laboratory, are examined by presenting field restoration data from several mining sites.

Jan 1, 1979

By H. H. Uhlig

IN our study of the mechanism of and the prevention of corrosion in stainless steels, it was considered of fundamental importance to obtain knowledge of the surface structure of such alloys. If corrosion resistance is due to a self-healing oxide layer, which like a paint film protects the underlying metal, it would be obviously relevant were the effort made to make the film less permeable and more adherent; for example, the surface might be expected to respond to an anodizing process, which is found successful in increasing the film thickness and corrosion resistance of aluminum. However, if passivity and corrosion resistance of stainless steels are due to another cause, the attack of the problem would follow another path. One of the most effective techniques for studying passivity and corrosion tendency is the measurement of the electrochemical potential. Not only can one determine by potential measurements whether a metal is active or passive, but also one can determine the degree of passivity and rate of transformation of passivity with time. Chemical media that build up or destroy passivity when in contact with the steel can also be classified by potential measurements. Something can be learned, too, of the effect of alloy additions such as molybdenum to 18-8, known to decrease corrosion of the alloy in chloride solutions. A study of alloys in previous investigations has sometimes included data on the electrochemical potentials. Tammann and Sotter1 measured the electrochemical potentials of alloys of iron-molybdenum and iron-chromium and reported the critical concentration of molybdenum or chromium at which passivity initiates. Strauss2 made similar measure-ments for the iron-chromium system. The electrochemical potential&apos; has also been used to indicate carbide precipitated 18-8. In 18-8, heat-treated to precipitate carbide, active metal exists at the region of the grain boundaries, contrasted with passive metal within the grains, the active metal accounting for a resultant active potential. Several

Jan 1, 1939

By E. Buehler, H. J. Levinstein

The temperature ranges in which the three inter-metallic phases in the Nb-Sn system form have been determined and the composition and structure of two of the three phases has been established. The kinetics of the formation of Nb3Sn in cored wire samples has been studied in the temperature range of 800° to 1050°C. From 800°to 950°C the rate of formation increases by four orders of magnitude. The rate-controlling step for the formation process in this temperature range appears to be the diffilsion of tin through NbSn. At higher temperatu~es a change occurs in the mechanism of the formation process such that up to a temperature of 1050°C the rate of formation of Nb3Sn does not increase above the rate observed at 950°C. For temperatures helow 950°C the current-carrying capacity of the wire increases with increased percent reaction reaching a maximum value when the formation process is 90 to 95 pct complete. The maximum current-carrying capacity obtainable in this temperature range is independent of the temperature. Above 950°C tlze current-carrying capacity obtainable in the wire decreases with increasing temperature of formation. A model is proposed which accounts for the ohserved behavior. RECENTLY, Buehler et a1.l reported the results of an investigation of the process variables which influence the superconducting properties of Nb3Sn-cored wire. These results indicated that at least four variables affect the properties of the manufactured wire. These include composition, particle size of the starting powder mix, temperature of heat treatment, and time of heat treatment. In order to understand completely the role of these variables, it is necessary to have an accurate knowledge of the phase equilibria in the Nb-Sn system. At the present time, phase-equilibrium diagrams for the Nb-Sn system have been published by a number of investigators.2-5 The diagrams differ as to the number of phases present, the composition of the phases, and the temperature range of stability of the phases. The present investigation was undertaken in order to resolve these differences. Since the investigation of Buehler et al. demon- strated that the length of time at the temperature of heat treatment affected the superconducting properties of Nb3Sn, it is apparent that it is necessary to understand the kinetics of the formation process as well as the equilibrium conditions before a complete understanding of the system is possible. As a result, the kinetics of formation of the various phases in the system were also studied in this investigation. EXPEFUMENTAL PROCEDURE Diffusion couples and sintered powdered compacts were employed in the phase-diagram investigation. The diffusion couples were made by filling 1/8-in.-ID monel-sheathed niobium tubes with tin. The monel sheath was employed to facilitate drawing.&apos; The tubes were then drawn to a tin-core diameter of 32 mils. Samples approximately 3 in. long were then cut from the drawn composite. The tin was drilled out of the ends to a depth of 1/4 in. and niobium-wire plugs were inserted into the ends and peened over. The monel was removed by etching in concentrated nitric acid, after which the samples were sealed in evacuated quartz bulbs and heat-treated in a resistance-wound tube furnace. The samples were quenched into ice water upon removal from the furnace. The diffusion couple samples were examined metallographically employing a chemical etching solution consisting of 10 ml of saturated chromic acid per g of NaF. In addition, two anodizing solutions were used for phase-identification purposes. The first was the picklesimer7 solution; the second consisted of equal parts by volume of 30 pct H2O2 and concentrated NH4OH to which 1 g of NaF was added per 25 ml of solution. The anodizing conditions for the second solution were 2 v and 100 ma with a tin cathode. The powdered compacts were made by pressing previously mixed powders of 99.9 pct pure Sn and 99.6 pct pure Nb supplied by the United Mineral Co. into cylinders 3/8 in. in diameter by 1/2 in. long. The cylinders were then sealed in quartz tubes and heat-treated in the same manner as the diffusion couples. The samples were examined metallographically and by X-ray diffraction techniques. Since it was desirable to be able to correlate the kinetic data with current-carrying capacity, the type of specimen chosen for this part of the investigation had to be a compromise between the optimum system for studying kinetics and one which was suitable for making current-carrying capacity

Jan 1, 1964

By L. D. Jaffe, H. C. Mann, E. L. Reed

It has been generally believed that fracture originates at a point and, if the stress is suficient, propagates across the material from this point. Evidence to the contrary is given in Fig 1. This micrograph shows an area close to the fracture of a steel containing The material had been quenched from 1675°F and tempered at 1150°F as a round about 10 in, in diam, and had a static tensile strength of 132,000 psi and a static yield strength of 105,000 psi. The steel was broken in 3000 cycles of reversed bending at a nominal max. fiber stress of 110,000 psi at a speed of 10,000 rpm. It was in the form of a standard R.R. Moore specimen with 45" V-notch, 0.015 in. radius and 0.220 in. diam at base of notch. The fractured edge in Fig 1 is part of the central portion of the specimen which broke during the final sudden fracture. Attention is directed to the short cracks which appear as dark lines within the specimen. Similar cracks were found in another specimen of the material, broken in 1,798,000 cycles at a nominal stress of 40,000 psi. The cracks were found in several areas close to the path of the final sudden fracture. This final fracture appeared microscopically to be wholly brittle and transcrystalline. Closer to the surface of the specimens, near the path of progressive fracture, which presumably advanced gradually during many cycles, there was microscopic evidence of some local deformation, but no microcracks. Neither were microcracks observed in areas distant from the main fracture path. The following explanation is offered: In the sudden fracture of the specimen, a crack propagates along a crystallo-graphic plane, with little or no plastic deformation of the adjacent material, until it reaches a grain boundary or a particle of carbide or inclusion which stops its advance. (The particle or boundary may be outside the plane of polish and not visible in the micrograph.) A stress concentration occurs about the end of the stopped crack. One or more new cracks are likely to start in the zone of this stress concentration. They may lie in the same grain as the first crack or in an adjacent grain. New cracks may occasionally start in a nearby but not adjacent grain whose orientation with respect to the stress leads to more ready fracture than does that of the grain between. Once started, these cracks propagate along crystallographic planes in their grains and the process repeats. This leads to discontinuous, branching chains of microcracks. As the process continues, microcracks probably tend to link up by fracture of intermediate material under the influence of increasing stress concentration. Occasionally, too, there may be a series of nearby grains of similar orientation so that there is a certain continuity of fracture across them. In either case the effective size of a crack is increased, resulting in greater stress concentration at its ends and a greater likelihood of further increase of size of the continuously-fractured region. When one continuous crack crosses the entire specimen, macroscopic fracture has occurred. The fractured edge of the specimen in Fig 1 represents a series of microcracks which became continuous across the entire specimen. The short, dark-appearing cracks in the figure did not become continuous over a large area. The row of microscopic stress concentrations at their ends may link up with those of the "main crack" outside the plane of polish. The above explanation does not imply that microcracks develop at the same rate in all portions of the specimen. They will develop most rapidly where the macroscopic tensile stress and macroscopic stress concentration are greatest. Viewed on a scale large compared to the grains, the fracture would appear to progress continuously across the specimen. Although Fig 1 shows a specimen broken in a fatigue test, it is believed that the microcracks discussed do not depend on the repetitive nature of the stressing used, since they are in the region where "sudden" fracture occurred, presumably in a single stress cycle. The whole process of microcrack propagation outlined above is thought to have occurred during this single cycle. It is believed that discontinuous crack propagation may be universal in brittle transgranular fracture of crystalline solids. Further experiments are under way.

Jan 1, 1950

By A. J. Langhammer

Broadly speaking, it may be said that the engineer has two major responsibilities: One is to recommend the choosing of proper machinery and equipment; the other, to assist in the simplification of design, determination of method, and advise about the most suitable material to be used. The products of powder metallurgy enter broadly into both these fields. The oil-cushion, self-lubricating bearing surface on a machine part makes for better machinery and factory equipment, often proves a life-saver in curing difficulties where bearings are overloaded or inaccessible for lubrication, or on installations that with normal practice constitute a problem entailing frequent repairs. On the other hand, other parts may require low porosity approaching solidity. In the second field, powder metallurgy provides many possibilities for improved products, improved performance, solving of technical problems, saving of weight, quiet operation, higher factors of safety, greater flexibility, attractive economies, and so on. Parts We of the automotive industries are making many powdered-metal war-machine parts, both ferrous and nonferrous, including gears, external and internal; ratchets, both external and internal; levers; pillow blocks; sliding blocks; cams; gibs; hubs with external and internal splines, and similar units. Powdered metals play an important part in our war work, as they did in peacetime in the manufacturing of passenger cars and trucks. The art of powder metallurgy is not a panacea. Although on certain parts such operations as turning, boring, facing, reaming, counterboring, milling, countersinking. chamfering, broaching, hobbing, profiling. trepanning, gear cutting, grinding, etc., can be eliminated, there will always be the need for machine tools. Advantages of Powder Metallurgy Simple machining operations often are eliminated by using powdered metal, and also many other intricate operations, some of which are of the type impossible to perform on the most modern production equipment; for instance, an external spline on a flange hub, where the spline must continue to the flange face and at full depth. Another important feature is that some of the machine parts may require a self-lubricating surface at one or more points; for example, proper lubrication of a sliding splined spool, while ordinarily most digcuit, is accomplished automatically with a self-lubricating powdered-metal bearing. Frequently machine parts are made with physical, mechanical and technological advantages unobtainable from cast or forged metals of similar analysis. Thus powder metallurgy offers the designing engineer broader latitude. Similarly, the engineer may take advantage of powder metallurgy in his teamwork with other departments. Another important advantage in powder metallurgy for machine parts is the relatively short time required for tool-up.

Jan 1, 1945

By M. S. Azun

I do not at all agree with the basic points of the author&apos;s conclusion. The use of lognormal or normal model to respond to the attribute distribution function should be carefully questioned. If fitting a distribution function of regionalized variables is the main purpose, one may employ one of certain well-known families of distributions, such as Tukey&apos;s lambda functions. For instance, the distribution function of gold assay values studied by Krige (Krige, 1978) may fit the lognormal model well, but one should not exclude that the basic idea of using the distribution function of observed data is to have insight of the physical mechanism that gives rise to the regionalized variables. In Applied Geostatistics, there are many examples considering only lognormal or normal model for the distribution function of geostatistical data even if the observed distribution function has more than one mode. Of course, using lognormal or normal model always brings easy computation for the statistical properties of attribute under investigation. Still, I object to adopting any of those models without having any "statistical inference." As seen from the author&apos;s paper, lognormal and normal model produce the same average grade (0.746% copper) and almost the same sample variance. Therefore, which model explains the probabilistic behavior of ore deposit is always an important question that should be replied by the geostatistician using not the common sense but the statistical and probabilistic methods. For kriging procedures, such as linear kriging, one should describe either second order stationary properties or bivariate properties of regionalized variables. Second order properties, such as correlogram function or semivariogram function, are the inputs of the so-called kriging equations. Selecting one of any useable models for the observed second order properties, such as spherical model, is not easy since the models are not based on the correlations structure of the regionalized variables. How those models being used in Applied Geostatistics can be distinguished is another important problem. One may develop many fitting models to respond to the observed second order properties of regionalized variables. However, I suggest that the model should be based on the probabilistic behavior of geologic process. The author used spherical model for copper, wolfram, and silver grades from isotropic sector (Fig. 2, 4, 3b) and exponential model for silver grades obtained along raises in isotropic sector (Fig. 3a). It seems that those semivariograms given in Fig. 3b for isotropic sector and Fig. 4 may be described by the random model implying that regionalized variables do belong to renewal process (Azun, 1983). If I knew the total number of data points used in estimation, may prove that my conclusion is correct. Recalling the test for the first order sample correlogram value, the test procedure is introduced such that the independence is rejected if [Ir(1) I > Za/2 N1/2] where Za/2 is the a/2 percentile of standard normal random variable and N is the total number of samples used in estimation (Azun, 1983). For the other observed semivariogram functions I suggest the author might try to use the so-called "Markovian model" describing not only the correlation structure of regionalized variables, but also the physical mechanism that produces the regionalized variables. The Markovian model for correlogram function is, [p (h) = T 1ih , h>1 ,] The Markovian model for the other second order properties of ReV are also derived. [T veß], in the above equation, show, for example, structural change and mineralizational variation in a considered deposit, respectively (Azun, 1983). In selecting any model, it is not easy to search for the "best" response to the observed second order properties of ReV&apos;s. The Markovian model, based on a theoretical understanding of underlying mechanism, gives more information about the occurrence of regionalized variables and respond to all properties. Random model and the so-called hole effect structure can be easily defined as a special form of the Markovian model (Azun, 1983). An estimation of any second order properties of regionalized variables may be computed through (N-1) lag. However, the dependency between the regionalized variables may be deemed to have "died out" after the so-called stationarity width (range). In practice, the estimation is carried out through 25% of the total number samples available. Therefore, the large fluctuations around the zero level and variance for correlogram or covariogram function and semivariogram function, respectively, cannot be observed. Since the number of pairs involved in the estimation of higher second order properties is small, the estimation variance at those lags is large. There is no need to show higher order estimated second order properties. After using one of any kriging procedure for block estimation, the distribution function of average grades has the same mean as the drilling sample grades but

Jan 1, 1986

By George G. Binder Jr., James W. Lacey, Arthur L. Draper

An experimental investigation of miscible fluid displacement has been made in linear porous media under highly adverse mobility ratio conditions. Various refined oils were displaced at field rates by liquid propane in both horizontal and vertical models 9 to 36 ft in length. In horizontal tests, mixed zones or transition zones form between the two liquids early in the displace-lents. Initially, the zones grow rapidly. III 2-in. diameter models, the mixed regions become nearly stable zones from 6- to 20-ft long. From then on these quasi-stable zones apparently grow only by molecular diffusion. The lenghts of the quasi-stable zones appear to be almost independent of the core material in which displacement;; are made and increase with increasing rates of injection and oil/solvent viscosity ratios. The lengths of the quasi-stable zones. measured in 2-in. diameter models at viscosity ratios and injection rates anticipated in the field indicate that essentially piston-like displacements of oil by solvent would occur. However, the mixed zone lengths increase markedly as the model diameter increases. In vertical displacements controlled by gravity drainage, only short trans-sition zones form. The entire lenghts of these zones can be accounted for by molecular diffusion. Therefore, in reservoirs having characteristics allowing a high degree of gravity drainage, nearly complete oil recovery should be attainable by miscible fluid displacement. INTRODUCTION The oil industry is faced with an ever increasing cost for finding new oil reservoirs. This, coupled with the fact that conventional methods of oil recovery usually leave from 1 to 3 bbl of oil in the ground for every barrel produced, has aroused considerable interest in developing more efficient methods. An integral part of the mechanism of many of these new methods of recovery is a miscible fluid displacement in which oil is displaced by a much less viscous materiai such as liquid propane. A numher of irlvestigators have explored the mechanics of miscible fluid displace-ment,&apos;.2.1.&apos;."." but in the experiments reported many of the important factors have been varied only over a limited range far removed from norma1 oilfield values. This paper presents the results of an experimental study of oil displacement by liquid propane at field rates from linear, natural-sandstone models of various sizes. Both horizontal and vertical flow tests were made. EXPERIMENTAL APPARATUS AND PROCEDURE Refined oils with viscosities varying over a wide range were displaced at several rates by liquid Propane from both horizontal and vertical flow systems. The behavior of the displacement was observed by propane-oil analyses of the effluent and, when possible, by differential pressure measurements along the cores. A schematic flow diagram of the apParatus used to conduct the experirents is shown in Fig. 1. The cores used in the tests were 9-ft lengths cut from natural consolidated sandstone and turned to the desired diameter. These were cast in steel tubing with a low melting point (160°F) alloy which expands on solidification. Flanges welded to the ends of the steel pipes permitted sealing the ends or butting one core to another. Pressure seals were maintained with O-rings. The cores were cleaned by flushing

By Fred E. Beasley

Metallurgists have, in the last ten years, overcome many difficulties of high zinc in lead blast-furnace slags. This problem was brought to the front at the close of the war, by the price obtained for lead and the high cost of labor, fuel, and flux. The Port Pirie plant of the Broken Hill Associated Smelters, Australia, early in 1919 had increased the zinc oxide in its blast-furnace slags from 13.5 to 20 per cent., at the same time reducing the iron oxide in the slag from 33.5 to 25.6 per cent. These results were obtained by the addition of 10 to 12 per cent. granulated slag to the roaster charge, improved conditions of the crushing, mixing, and roasting of the constituents of the sinter. By experiments and improvements, the practice at this plant has developed a normal slag that carries 22 per cent. zinc oxide, and at times runs as high as 33 per cent. zinc oxide, with only slight furnace trouble. The granulated slag is used not only as a diluent to the sulfur in the roaster charge, but on account of its value as a slag-forming material and the physical properties it imparts to the finished sinter. The ore is mixed with flux and given a double roast. All the first roasting is by sintering with the Dwight & Lloyd machines. The final roasting is performed partly by Dwight & Lloyd machines and partly by H. & H. pots. The charge to the blast furnace consists chiefly of the final sinter, slag shells, siliceous and non-bearing sulfur lead ores. High blast and ore columns are the practice. The greatest care is taken to obtain in the final sinter as low a sulfur content as possible. Attracted by the success of the Port Pirie plant, The Consolidated Mining & Smelting Co. of Canada, at Trail, B. C., in 1920 treated its crushed primary sinter with about 15 per cent. granulated slag. The Trail smelter at this time was short of ore and a large part of the charge to the roasters consisted of the zinc-plant residue having the following analysis: 12 to 16 per cent. lead, 12 to 16 per cent. zinc, and 25 to 30 per cent. iron. The lead in the final sinter was low and the physical condition was so bad that all the sinter had to be screened before it could be charged to the blast furnace. Also it disintegrated on being trammed and dumped

Jan 1, 1925

By G. W. White

Over the past several years, the steady progress of gas lift from a mysterious art into a developing science has been traceable through the many fine papers that have appeared in Journal of Petroleum Technology. Consequently, this magazine has rightly become a standard for the serious students of gas lift all over the world. The following discussion is offered in a sincere attempt to accurately present certain topics covered in the subject paper in the light of acknowledged state of the art procedures. INSTALLATION DESIGN The first point to be questioned is the author&apos;s installation design, beginning with Eq. 6. The use of 1,200 psi in the spacing equation instead of the 1,275 psi noted as available seems, at first glance, to be a simple arithmetic error. Upon further examination, it appears evident that both this 75 psi plus the 100-psi safety factor must be subtracted from available kickoff pressure because of conditions imposed by the characteristics of the ASC valve (see Fig. B-1). Pressure-charged valve design is incorrectly penalized by spacing the first valve using only 1,100 psi. The use of such a high back-pressure makes it appear that a typical ASC installation would require no more valves than a comparable conventional valve installation. Using a value of 100-psi tree pressure, the well could be valved to 11,000 ft very conservatively with seven pressure-operated valves, but would still require 11 ASC valves. The use of 400-B/D spacing gradient for a 140-B/D rate is not an accepted practice using precharged valves. The author would have done well to note the advantages to be gained by reducing the 500-psi tree pressure, which is clearly explained by Beadle, Harlan and Brown.&apos; In Step 1 of Part III of the continuous flow discussion, the author incorrectly applies the Poettmann and Carpenter curves.2 Item 2 is an incorrect statement. An excellent reference on this point is the paper by Baxen-dell and Thomas.&apos; VALVE MECHANICS The next topic relates to the mechanics of precharged valves. Eq. 2 for the ASC valve can be used to describe the condition of equilibrium, wherein the valve is closed with opening pending. When this equation is used to determine relative values of casing, dome and tubing pressure with conditions approaching the transition value, some strange results are obtained. The following uses the author&apos;s symbols and values given on page 689. Fig. B-1 shows the condition that exists at the moment an ASC valve has been uncovered during the unloading process (Condition I). The obvious result is a locked condition. The basis for the curve is shown on the figure which includes 1,000 psig casing pressure to uncover the valve. If injection gas is not bled off the casing until the pressure is decreased by an amount exceeding the stabilizer discharging valve pressure, upward adjustment of the casing pressure is mandatory for the valve to open and unloading operations to continue. In Condition I the dome pressure exceeds the casing pressure by 20 psi, and the tubing pressure required to open the valve is 1,212 psig. This tubing pressure would not exist under the assumed conditions. In Condition I1 the casing pressure is increased to the dome pressure, and the tubing pressure required to open the valve is 1,102 psig. It is apparent that the casing pressure must be increased to a value exceeding the dome pressure before unloading operations could continue. In Condition I11 a maximum casing pressure of 100 psi (stabilizer charging valve set pressure) above the dome pressure is reached, and the tubing pressure required to open the valve is 549 psig. The author&apos;s statement after Eq. 5 that "the minimum tubing pressure required to open an ASC valve is equal to the casing pressure at depth less the transition pressure of the valve" is incorrect except for Condition I11 only. Otherwise, the equation is invalid.

Jan 1, 1965

By D. Perry, G. W. Binkley, G. K. Dumbauld, F. A. Brooks

A new cementing technique has been developed which is particularly applicable to permanent-type well completion operations. The technique makes use of the accelerating effect of calcium chloride on setting time and strength development of cement cake deposited in squeeze cementing. An unique feature is that the accelerator is applied after the unaccelera-ted cement slurry has been squeezed and the excess has been reversed from the well. Laboratory data on the accelerating effect of calcium chloride applied to the fi1ter cakes of three low-water-loss cementing compositions demorzstrate that the procedure results in relatively rapid development of strength and impermeability of the cement cake. Simulated squeeze-ceinenting tests made in the laboratory likewise corroborated the practicality of the procedure. The laboratory tests showed that a newly developed oil-emulsion cemerzting composition is more susceptible to acceleration of set than are modified cements containing high percentages of bentonite. The acceleration procedure has been used successfully in field operations. INTRODUCTION Nature of Problem In squeeze-cementing operations, a substantial amount of time is consumed in waiting on the cement to develop strength after it has been squeezed into the well. Frequently, an interval of 18 to 24 hours or longer is required for the development of strength sufficient to prevent failure of the cement during subsequent operations in the well. Reduction of this waiting-on-cement time offers appreciable savings both in time and in money. A particular type of squeeze-cementing operation to which an increasing amount of attention has been given is encountered in permanent-type well completion operations wherein perforations are to be squeezed off1. In this procedure, it is customary to pump the cement slurry down the tubing and out into the perforated section through a retractable extension pipe. Squeeze pressure is then applied, which forces the cement slurry into the perforations and causes the build up of a compact filter cake of cement within the perforations. The excess slurry remaining in the hole is then removed by reverse circulation. The extension pipe is then retracted, and, if a new interval is to be perforated, a perforating gun is run through the tubing. The newly perforated interval may then be tested by swabbing. In such operations, it has been customary to allow approximately 20 hours or so for hardening of the cement squeezed into the perforations. This time interval is usually measured from the time that the cement is reversed out of the hole to the time that subsequent swabbing is started. If the cement has not developed strength at the commencement of swabbing, the pressure differential caused by swabbing results in failure of the squeeze job. At the time that the work described in this report was initiated, particular consideration was given to the reduction of waiting-on-cement time in squeeze cementing by the permanent-type completion technique. Consequently, much of the experimental work was directed to this specific objective, though the process which was developed for acceleration of strength development has possible application in other than permanent-type completion operations. Method of Attack Although quick-setting cements

Jan 1, 1957

By H. C. Fiedler

A high degree of cuhe-on-edge grain orientation and good magnetic properties were obtained in Si-Fe strip processed from laboratory heats containing vanadium nitride inclusions. The higher the nitrogen content the greater was the restraint on normal grain growth and the greater was the ability to undergo secondary recrystal-lization. The degree of restraint in a heat containing magnanese sulfide inclusions was slightly greater than that in the lowest nitrogen vanadium nitride heat. The high rate of diffusion of nitrogen in the temperature range in which the texture is developed makes it necessary to retard the loss of the inclusions until the texture has been developed. MAY and Turnbulll have shown that to develop the cube-on-edge secondary recrystallization texture in Si-Fe it is necessary that inclusions, such as manganese sulfide, be present to prevent normal grain growth. They showed that the driving force for the growth of the secondary grains is inversely proportional to the diameter of the matrix grains, and that the function of the inclusions is to maintain a small matrix grain size. Fast3has developed cube-on- edge texture in Si-Fe by nitriding the hot rolled band. The silicon nitride thereby formed promotes secondary recrystallization during the anneal of the final gage strip. To obtain the best magnetic properties, the inclusions must be removed from the strip after the grain orientation has been developed. Nitride inclusions have an inherent advantage over sulfide inclusions in that the greater diffusivity of nitrogen as comared to sulfur permits the use of shorter times and or lower temperatures for the purification heat treatment. The purpose of the work to be described was to examine the usefulness of vanadium nitride inclusions in developing the cube-on-edge texture and to determine the magnetic properties of oriented strip made from heats containing these inclusions. A comparison is made with a heat having had iden-

Jan 1, 1962

By Nicholas J. Grant, A. W. Mullendore

Measurements of grain boundary sliding were made on polycrystal and bicrystal tensile creep specimens of Al-2 pct Mg at 500oand 700oF. Grain and pain boundary orientation factors were studied with respect to their effect on the magnitude and direction of grain boundary sliding. It was concluded that a large part of the observed sliding may be caused by the operation of slip crossing the grain boundaries. Supporting evidence for this model from other investigations is also given. GRAIN boundary sliding in metals during elevated temperature deformation has frequently been thought of as an independent mechanism with its own characteristic stress, temperature, and structure dependence. Further, it is common to regard the grain boundary as the weak link during creep deformation since: 1) the strength of apolycrystallinemetal, as meas-sured by creep rate or rupture life, decreases at\a more rapid rate when sliding comes into action, and 2) grain boundary sliding, as revealed by "boundary darkening" and fold formation is often the first visible deformation. On the other hand, more quantitative observations, in both polycrystals and bicrystals, have shown boundary deformation to be closely related to the over-all deformation of the specimen. The curve of grain boundary contribution to elongation vs time takes a shape similar to that of the total creep curve,&apos;,&apos; and the apparent activation energy for sliding appears in most cases to have the same value as that for total creep.3 In order to reconcile these observations, one is left with these possibilities: 1) The grain boundary and grain deformation rates are both controlled by the same rate limiting processes. 2) The rate of sliding is limited by accommodation deformation in the grains. 3) Sliding is the consequence of grain deformation. 4) Grain deformation is dependent on prior grain boundary deformation. Alternatives 2) and 3) would view grain boundary sliding as occurring in series with another deformation process which could be rate controlling. McLean prefers item 3) as the sliding basis,4 where subgrain rotation results from dislocation accumulation in the substructure at the grain boundary. Crussard and Friedel&apos;s5 treatment of grain boundary migration considers that dislocations are forced into the grain boundary and are dissociated into dislocations with Burgers&apos; vectors nearly parallel to the grain boundary. The movement of these partial grain boundary dislocations then produces the sliding. The results of this investigation have indicated alternative 3) to be the most appropriate and it is this aspect of grain boundary sliding which will be analyzed. EXPERIMENTAL PROCEDURE Three types of tensile creep tests were employed in this study: (I) A constant load test of one very coarsegrained polycrystalline specimen at 500° F, 3600 psi, 1 pct per/hr strain rate to examine the grain and grain boundary orientation factors in grain boundary sliding. (II) Constant strain rate tests of polycrystalline specimens at 510o and 715o F, 2 pct per/hr strain rate to determine the grain boundary contribution to elongation at very low total strains. (m) Constant strain rate tests of bicrystals of various grain and grain boundary orientations at 500°F, 2 pct per/hr strain rate to obtain further information on the orientation effects in grain boundary sliding. The material used in the tests was a high-purity Al-1&apos;.92 mg alloy, kindly furnished by Alcoa. Its composition is given in Table I. The alloy is a solid solution at the test temperatures. The coarse grained polycrystalline specimen for test (I) was prepared by recrystallizingthe machined specimen, straining it about 1pct intension at room temperature and annealing at 900°F for 8hr. The constant strain rate specimens (11), with an 178 in. sq. by 1/2 in. long gage section, were cut from 1/8 in. thick sheet of cold rolled and annealed (8 hr at 1000oF) material. The latter specimens were supported in a special jig during the milling operations to avoid any bending, and the gage section was subsequently heavily electropolished to remove the cold-worked surface layer. The bicrystals (ID) were machined in the same

Jan 1, 1963

By G. Venturello, C. Antonione, G. Della Gatta

Results from work on the effect of inferstitials on recovery and recrystallization of&apos; very pure iron (99.995 pet) doped with nilrogen up to 400 ppm are reported. Nitrided specimens were obtained by heating the iron in a static atmosphere of NH3 + H2. The samples were cold-rolled 80 pet, subjected to a series of isochronal and isothermal anneals, and submitted to examination by X-rays, micrographs, and hardness tests. Small additions of nitrogen show a strong effect in reducing recovery of&apos; the mechanical properties of high-purity iron. At the temperatures of. the experiments, this effect proved greater than in the case of carbon. At 400°C pure iron recovers more than 50 pet of the total hardness increase, carburized iron vecovers 25 pet, and nitrided iron only 10 pet. On the other hand. the addition of nitrogen has, similarly to carbon, a very small effect on recrystallization; the effect is, however, slightly higher than that of carbon. When the concentration Of nitrogen is above the solubility limit in a iron at the temperattue of the experiments, an increase in the frequency of nu -cleation is also observed. THE object of the present work is to improve knowledge on the effect of interstitials both on recovery and on primary recrystallization of pure iron. In fact. at present there are no available data on the effect of nitrogen on high-purity iron. The only work which at present can be somewhat related to this problem is a work of Leak et al.1 in which grain boundary internal friction at high temperature in the presence of increasing amounts of nitrogen is studied by a torsion pendulum. The present work is a continuation of a previous one2 on the effects of carbon. EXPERIMENTAL PART Preparation of the Material. Pure iron was prepared following the same methods used in the pre- vious work2 and was nitrided using controlled quantities of ammonia in an apparatus similar to that used for carburizing. The apparatus consists essentially of a gas-tight quartz tube containing the specimens. The tube, maintained at constant pressure by means of a mercury seal, is placed in a resistance furnace. For nitriding, the NH3 + H2 atmosphere with a suitable concentration of NH3 was introduced into the tube, which had been previously carefully evacuated and degassed by heating at 600°C. The hydrogen used was carefully purified by passing it through a palladium filter. The ammonia required was prepared with the following reaction: CaO + 2NH4CI —CaCl2 + H2O + 2NH3 by heating the mixture of CaO and NH4C1 in a glass flask and then collecting the ammonia in a graduated Hempel burette. For each nitriding program a given amount of NH3 prepared by this method was introduced together with the H2 into the tube previously evacuated. Nitriding of the sample was then performed at 570°C for 48 hr. After this, to ensure a homogeneous distribution of nitrogen, the samples were further heated for 72 hr at 800°C. With this method which uses a static nitriding atmosphere, carefully controlled conditions of purity are obtained. Contrarily, with the conventional continuous-flow methods, using large quantities of circulating gas, there is a greater risk of introducing impurities into the samples. Furthermore, the required nitrogen concentration in the specimen is easily predetermined and obtained. A plot of the relation observed between the initial concentration of NH3 in the gas and the quantity of nitrogen introduced into the iron samples is given in Fig. 1. The data refer to samples of 1.2-mm thickness and to the nitriding conditions previously described. Furthermore, as a comparison, the data relative to two 0.5-mm-thick samples are reported. The presence of a reservoir in the cold zone of the reaction bulb made possible the gradual dissociation of ammonia on the sample in the hot zone. Internal-friction methods were used to determine the content of nitrogen dissolved in the iron samples. Some analyses were also carried out with chemical methods. The following table, Table I, shows a comparison of data obtained with chemical and internal-friction methods. The correspondence between chemical methods and internal-friction

Jan 1, 1964