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By Howard E. McKinney

A high-pressure wellhead lubricator has been developed to facilitate telemetering electrical measurements from subsurface reservoirs to the surface with the well under normal flowing conditions. The field unit in use at the present time employs a 5/16-in diameter, single-conductor armored cable and is to be used in wells with surface pressures up to 5,000 psi. It has a pressure sealing element that maintains a continuous and absolute seal around the cable as it enters or leaves the tubing at speeds up to 175 ft per minute. A cable injecting device is used which obviates sinker bars or weight sections on the instrument. INTRODUCTION The development of instruments for securing physical measurements in pressure wells has been confined in the past to those instrument which would operate on a wire line and record the necessary measurements in the downhole instrument itself, or those which would operate on an electric cable in a well with the surface pressure killed by the use of weighted fluids or by the use of tubing plugs. In one case the accuracy of the measurements is questionable, and in the other the range of application is very limited. Considerable work has been done by other interests to provide effective means to accomplish the necessary telemetering. The U. S. Bureau of Mines developed a wellhead lubricator prior to 1947 which permitted a 5/16-in diameter single-conductor cable to be lowered into a well with a surface pressure of approximately 500 psi. This unit was used successfully in a number of tests in Oklahoma. A company which tests wells has recently offered on a service basis a wellhead lubricator with a 3/16-in diameter cable that reportedly operates up to 2,500 psi surface pressures. Each of the above operates on a staging principle to effect a seal. In both of these units some leakage of well fluid occurs when the cable is moved. SPECIFICATIONS FOR DESIGN In order to provide the maximum flexibility in its use, the following parameters were established for the design of our high-pressure wellhead lubricator: L An absolute well fluid seal up to 5,000 psi surface pressures. 2. Means for raising and lowering the instrument at speeds of at least 100 ft per minute. 3. Provision for the instrument to enter and leave the well without disturbing the well flow or the reservoir conditions. 4. A cable large enough to provide suitable electrical characteristics and suitable mechanical properties. 5. A method of operation that will not damage the well in any way. The present high-pressure wellhead lubricator field unit fulfills the above requirements. DESCRIPTION OF THE UNIT AND ITS OPERATION The cable selected for this use is the standard Amergraph 1H2 as manufactured by the American Steel and Wire Co. This particular cable is normally used by the Halliburton Oil Well Cementing Co. in their conventional well logging operations. Although the cable presents a noncircular cross-section (Fig. l), its diameter is very consistent; lor example, maximum diameter is 0.325 in., minimum diameter 0.314 in. This [actor permits the use of the sealing element, as later described. Early in the development of the high-pressure wellhead lubricator it was apparent that we could not effect a direct gas seal around a moving 1H2 cable. This becomes evident when an examination of the cable cross-section is made. The voids between the strands of the outer armor provide natural channels lor the flow and escape in large quantities of a low-viscosity fluid such as gas. However, it is relatively simple to

Jan 1, 1952

By J. E. Miller, W. E. DeVaney, L. Stroud

During a recent phase study of a natural gas, two stable equilibrium liquid phases were observed at temperatures below —200°F and pressures above 200 psi. This paper reviews the published literature on the occurrence of multiple equilibrium liquid phases and presents analytical data for the vapor and two equilibrium liquid phases of the liquefied natural gas at five experimental conditions. In addition, data for 30 conditions of two-phase equilibria are included. INTRODUCTION The low-temperature phase behavior of gases, most of which contained helium, has been investigated in the laboratories of the Helium Activity for many years. Since 1952, experimental studies of these systems have been continuous as part of the research program at Amarillo, Tex. Because of their value to private industries interested in participating in the Helium Conservation Program, several "Open File" reports containing phase equilibria data for heliurn-bearing natural gases have already been released by the Helium Activity. A paper containing information on the general phase behavior, operating criteria and extensive vapor-liquid data for two helium-containing systems was recently published.2 Additional publications presenting experimental data on the phase relationships of various gas systems are now in process and will be available in the near future. PREVIOUS EXPERIMENTAL WORK Although the formation of multiple liquids has been reported for various systems, to our knowledge this paper is the only substantiated evidence of a vapor-liquid-liquid equilibria in a naturally occurring gas. In 1940, Vink, Ames, and others13 reported the presence of two liquid phases in a hydrocarbon system consisting of mixtures of crude oils, solvents and natural gas. Eilerts and co-workers; published data on the recombined fluids from a gas-condensate well. This condensed gas, containing approximately 76 per cent methane and 24 per cent ethane-plus, exhibited two distinct liquid phases. Weinaug and Bradley 14 observed "unusual" phase behavior in a reservoir mixture. These workers postulated that the anomalous phase behavior was due to the "imminent formation of a second liquid phase". Botkin, Reamer, Sage and Lacey 1 studied two California crude oils that exhibited multiple phases. Kohn and Kuratal0 recently reported two equilibrium liquid phases in the methane-hydrogen sulfide system. Roof and Crawfordl1 and Eakin, et a16 also have reported experiments with binary systems that formed two stable equilibrium liquid phases. APPARATUS AND PROCEDURE A U. S. Bureau of Mines Phase Equilibrium Apparatus was used in conducting this study. The apparatus and procedures employed in its operation have been previously described3 and will not be repeated in detail ill this report. Briefly, the apparatus consists of a windowed cell which can be maintained within ±0.5°F for temperatures between room temperature arid -320°F. Pressure within the cell can be maintained within 0.1 per cent of gauge reading up to 800 psig. Equilibrium vapor and liquid samples are obtained in special containers4 for analysis by a mass spectrometer. Although the accuracy of the analyzer is about ±0.1 mol per cent, the reproducibility of the phase-equilibrium apparatus is considered relatively poor. Values reported from methane and nitrogen are considered accurate to ±l.0 and ±0.6 mol per cent. Data for ethane-plus in the vapor are accurate within 0.2 mol per cent; liquid-phase data for this aggregate compolnent are accurate within 1.5 mol per cent. For helium in the vapor phase, the analytical data are accurate within 0.2 mol per cent; liquid-phase analyses for this component were obtained by the charcoal adsorption method described by Frost8 and are accurate within 0.006 mol per cent. All of these references to the accuracy of reported values are conservative estimates based upon a statistical treatment of reproducibility data obtained with the apparatus.

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. 'The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,' In-AS,' and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956

By Philip R. Strand, O. F. Stewart

Vermiculite is the name generally applied to the group of hydrated ferromagnesian aluminum silicates that are characterized by the ability to expand when heated. This process, called exfoliation, results in a lightweight product of commercial value. Most uses of vermiculite are for the expanded material. The chief markets are in construction, agriculture, and horticulture, with lesser uses in general industry. Composition and Properties Vermiculite, in its natural state, has the characteristic micaceous habit, a perfect basal cleavage which causes splitting into thin laminae that are soft, pliable, and inelastic. The structure of vermiculite is basically that of a talc. The prominent monoclinic crystal faces are often marked by lines at 60° and 120°. Hardness varies from 1.5 to 2 or more; specific gravities are between 2.1 and 2.8; color varies from almost clear to amber, bronze, brown, green, or black. Vermiculite feels like talc, especially when wet. Although much research has been performed on the chemical and structural composition, there is not yet complete agreement on the exact formula. This is to be expected when different workers have examined the many different varieties. Vermiculite is not considered to be a single mineral species but a family of related minerals. The structural formula for a trioctahedral vermiculite may be written: (H20)-(Mg,Ca,K)-(A12,Fe,Mg)-(Si,A1,Fe)4O10 (OH) 2 Hydrobiotite also occurs with vermiculite and is usually considered a vermiculite for commercial uses. When heated quickly to elevated temperatures, vermiculite expands by exfoliating at right angles to the cleavage into wormlike particles. The name vermiculite is derived from the Latin vermiculare, to breed worms. This characteristic of expansion is the result of the mechanical separation of the layers by the rapid conversion of contained water to steam. The decrease in bulk density of commercial grades is usually approximately 10 times, from 50 to 5 lb/ft3, but varies depending on the quality, size, and furnace efficiency. Individual flakes may expand up to 30 times. Vermiculite may also be expanded by soaking in chemicals such as hydrogen peroxide, weak acids, and other electrolytes. Color change during expansion is dependent upon the type of vermiculite and furnace conditions. Heating in an oxidizing atmosphere produces a dull gray or tan color, whereas a reducing atmosphere can produce a bronze or gold color. The expansion of the vermiculite crystal results in large pores being formed between the platelets. Thus, exfoliation makes available a large increase in void volume which is important in the application of vermiculite as a chemical carrier. Mathieson and Walker (1954) state vermiculite must be regarded as a true clay mineral. The characteristic properties of the mineral, such as high cation exchange capacity, organic complexing ability, and variable interlamellar distance are very similar to those of montmorillonite. The cation exchange capacity of vermiculite is one of the highest of all the clay minerals. The interplatelet space is accessible to penetration by some electrostatically neutral molecules. Water and glycerine are two common substances whose molecules may be so imbibed. In the natural state and under normal atmospheric conditions, water occupies the spaces between the silicate layers. The crystal d-spacing is near 14.2A. By differential thermal analysis, it has been determined that the water

Jan 1, 1983

By G. Ansell, J. Weertman

G. Ansell and J. Weertman (Rensselaer Polytechnic Institute and Northwestern University, respectively) —The great increase in creep strength that you found in your indium-glass composites is quite striking. You ruled out a decrease in the dislocation source density as an explanation of the reduced creep rates. Could you tell in greater detail why you feel this is an inadequate explanation of the phenomenon. It appears to us that it is a reasonable one. Consider the spacing between the glass spheres in your composites. It is of the order of 10-3 cm. The spacing between dislocations in a (single-phase) annealed metal with a dislocation density of the order of 106 to 107 cm per cm3 also is of the order of 10-3 cm. Therefore it is not reasonable to expect that the arrangement of the dislocation lines is the same in the composite material as it is in pure indium. If the dislocation arrangements are different the density of the dislocation sources likewise will be different. Another way of saying the same thing is the following. The presence of the glass spheres reduces one of the dimensions of the metal phase to 10-3 cm. Thus the metal phase, in effect, is equivalent to a metal whisker or a thin metal film. These are strong because they have so few dislocation sources within them. T. D. Gulden and J. C. Shyne (authors' reply)—It is to be expected that the arrangement of dislocations in the indium-glass composites would be quite different than that observed in annealed pure metals. The dislocations probably exist primarily as segments connecting the dispersed particles. These segments and discontinuities at the very large area of particle-metal interface could act as dislocation sources. For this reason it was considered unlikely that the very high observed creep strengths were due to a low density of dislocation sources. A more likely explanation is that the distance a dislocation can glide is limited by the interparticle spacing. The particles averaged about twenty in diam and were less than 10 µ apart in the 40 pet composite. It seems reasonable to assume that a dislocation loop in a volume of metal surrounded by these relatively large particles would not bow out around them but would be restricted to the region between particles. A general expression for creep rate is given by the product of the dislocation source density, the average rate at which loops are generated from a source, and the average area swept out by a loop times the Burgers vector magnitude. Assuming that the area swept out is limited by the interparticle spacing and the rate of generation of loops is controlled by the rate of climb of loops over second-phase particles, as suggested by Ansel and Weert-men,9 a calculation of the dislocation source density may be made from the experimentally observed creep rates. The result comes out 10" to 10" per cm3 which seems reasonable in view of the assumptions involved. Thus it is concluded that the anomalously low creep rates that were observed were due not to a low dislocation source density but rather to a limitation on the area swept out by each dislocation loop.

Jan 1, 1964

By M. A. Dayananda, R. E. Grace, P. F. Kirsch

Ternary diffusion experiments were carried out at 750°C with vapor-solid diffusion couples in single-phase copper-rich Cu-Zn-Sn alloys. The Philibert-Guy method was used to calculate intrinsic diffusion coefficients at compositions corresponding to the plane of inert markers imbedded in the diffusion couples. Inter diffusion coefficients were determined at common composition points of intersecting diffusion paths. Intevdiffusion coefficients were also obtained at compositions corresponding to maxima in the tin concentration pvofiles Relations between the interdiffusion coefficients and the expansion of vapor-solid diffusion couples are described in detail. Such relations permit the calculation of constant interdiffusion coefficients in binary couples from expansion data directly. In ternary couples expansion data provide an additional constraint on the interdiffusion coefficzents. ThE phenomenological analysis of diffusion in ternary solid solutions has been developed extensively, and various approaches taken in the determination of diffusion coefficients have been reviewed recently by Guy et al.' Finite,' semi-infinite,3 and infinite4 diffusion couples have been used in studies of ternary diffusion, but most of the work has been done with infinite diffusion couples. Semi-infinite diffusion couples3 (vapor-solid couples) have been used to determine both intrinsic and interdiffusion coefficients in the Cu-Zn-Mn system, in which two diffusing species, zinc and manganese, were supplied from the vapor phase. If only one component has a sufficiently high vapor pressure to be supplied from a vapor source, vapor-solid diffusion couples may still be used. In this case the boundary conditions at the gas/solid interface may be governed by partial equilibria rather than by virtually complete equilibrium between the phases. In the present work diffusion measurements were carried out at 750°C with vapor-solid couples of Cu-Zn-Sn alloys. Only zinc was transported between the vapor source and the diffusion disks, because the vapor pressures of both copper and tin are at least 108 lower than that of zinc. Both intrinsic and interdiffusion measurements were made at several compositions. A secondary objective was to relate expansion of the diffusion couples with the interdiffusion process. Such measurements for binary couples yield average values of the interdiffusion coefficients over composition increments. In ternary diffusion couples ex- pansion data provide an additional constraint on the interdiffusion coefficients. COMPOSITION-DEPENDENT INTRINSIC AND INTERDIFFUSION COEFFICIENTS As shown by Philibert and GUy5 the determination of intrinsic diffusion coefficients in a ternary system requires two independent diffusion couples containing marker planes with identical composition. In the case of vapor-solid couples such a requirement torresponds to two couples set up with the same vapor source exposed to two diffusion disks of different composition. Inert markers placed initially on the disk surfaces become imbedded during diffusion. If the pair of couples exhibits appreciable marker burial with marker planes of virtually the same composition, the intrinsic diffusion coefficient may be evaluated at the composition of the marker planes. Fig. 1 is a schematic diagram of the concentration of of a Cu-Zn-Sn ternary vapor-solid couple after diffusion of zinc from a vapor source into a binary Cu-Sn alloy. The areas, Ai correspond to the cumulative intrinsic fluxes of the three diffusing species across the marker plane:5 where Ji is the intrinsic flux of component i, t is the diffusion time, and D3i are the intrinsic diffusion coefficients. For the determination of interdiffusion coefficients a pair of diffusion couples with intersecting diffusion paths is needed. At the composition point of intersection (C1, C2) the coefficients are evaluated from the equation:3

Jan 1, 1969

By R. Q. Shotts

Data are presented which show that fractions of varying densities from the same coals are oxidized at different rates by nitric acid. From oxidation data, the approximate quantity of "bright" and "dull" components may be calculated. Definite relationships between oxidation rate and rank are shown for density fractions from at least two bituminous coals. IN 1945, the Alabama State Mine Experiment Station initiated a program on the determination of fusain in certain coals of the state.1 Because of the lack of equipment and personnel necessary for microscopic examination, the chemical method2 was used exclusively. During studies of the distribution of fusain in fractions of various sizes and densities on a medium volatile coal, the author noted a higher rate of oxidation of the nonfusain part of the coal in the lower density fractions and the difference in rate became more marked the shorter the oxidation period used. Since durain and other "dull" components of coal have been reported3,4,5 to have higher densities than vitrain and the bright components, it appeared probable that the observed differences in rates of oxidation in the different density fractions were due to variations in petro-graphic composition. Such effects have been noticed by other workers.2,3 In order to obtain further evidence on this point, several Alabama coals of different rank have been separated into three or more fractions on the basis of density and their rates of oxidation determined, using the procedure specified for the determination of fusain, except that measurements were made at short time intervals as well as for the longer periods specified in the regular procedure. Significant differences in the rates of oxidation of the nonfusain part of the various fractions have been observed, and it is believed that studies of this type may make possible the identification of individual petrographic components or lead to methods for their semiquan-titative estimation. Properties of the Coals: Analyses and some properties of the whole coals studied are given in table I. The range in rank of the coals is not the widest possible within the state, but samples of the low volatile coals that occur in thin beds in the northeastern part of the state, were unavailable. The Clements bed is not, at present, considered workable. The coal is of medium volatile rank, quite friable, and very strongly swelling. Analyses of different size fractions show that the larger sizes are of higher rank than the smaller ones. Material passing the No. 50 sieve (all sieve sizes refer to the U. S. Standard Series) is close to high volatile A in rank, except for the size passing a No. 200 sieve, in which fusain is partially concentrated. Because of the variation in rank of the sizes of Clements coal, oxidation studies were made of two widely different size ranges. The + 1-in. material was crushed on rolls to about 1/8 in. and separated into five fractions by float-and-sink treatment in a benzene-carbon tetrachloride mixture. The — No. 4 + No. 8 and the — No. 4 + No. 50 size ranges tested overlap but the latter size was studied last with the expectation that it would include more oxidizable material than the first size. This proved not to be the case. Yields and properties of the specific gravity fractions oxidized are shown in table II. Milldale bed coal probably represents, as nearly as it is possible to do so, the "average" coal of the state. The material passing a No. 4 sieve was the only size range oxidized. It was divided into four specific gravity fractions. As in every case the heaviest fraction, which was essentially rock, was discarded. The Black Creek is the most extensive in area of

Jan 1, 1951

By R. Q. Shotts

Data are presented which show that fractions of varying densities from the same coals are oxidized at different rates by nitric acid. From oxidation data, the approximate quantity of "bright" and "dull" components may be calculated. Definite relationships between oxidation rate and rank are shown for density fractions from at least two bituminous coals. IN 1945, the Alabama State Mine Experiment Station initiated a program on the determination of fusain in certain coals of the state.1 Because of the lack of equipment and personnel necessary for microscopic examination, the chemical method2 was used exclusively. During studies of the distribution of fusain in fractions of various sizes and densities on a medium volatile coal, the author noted a higher rate of oxidation of the nonfusain part of the coal in the lower density fractions and the difference in rate became more marked the shorter the oxidation period used. Since durain and other "dull" components of coal have been reported3,4,5 to have higher densities than vitrain and the bright components, it appeared probable that the observed differences in rates of oxidation in the different density fractions were due to variations in petro-graphic composition. Such effects have been noticed by other workers.2,3 In order to obtain further evidence on this point, several Alabama coals of different rank have been separated into three or more fractions on the basis of density and their rates of oxidation determined, using the procedure specified for the determination of fusain, except that measurements were made at short time intervals as well as for the longer periods specified in the regular procedure. Significant differences in the rates of oxidation of the nonfusain part of the various fractions have been observed, and it is believed that studies of this type may make possible the identification of individual petrographic components or lead to methods for their semiquan-titative estimation. Properties of the Coals: Analyses and some properties of the whole coals studied are given in table I. The range in rank of the coals is not the widest possible within the state, but samples of the low volatile coals that occur in thin beds in the northeastern part of the state, were unavailable. The Clements bed is not, at present, considered workable. The coal is of medium volatile rank, quite friable, and very strongly swelling. Analyses of different size fractions show that the larger sizes are of higher rank than the smaller ones. Material passing the No. 50 sieve (all sieve sizes refer to the U. S. Standard Series) is close to high volatile A in rank, except for the size passing a No. 200 sieve, in which fusain is partially concentrated. Because of the variation in rank of the sizes of Clements coal, oxidation studies were made of two widely different size ranges. The + 1-in. material was crushed on rolls to about 1/8 in. and separated into five fractions by float-and-sink treatment in a benzene-carbon tetrachloride mixture. The — No. 4 + No. 8 and the — No. 4 + No. 50 size ranges tested overlap but the latter size was studied last with the expectation that it would include more oxidizable material than the first size. This proved not to be the case. Yields and properties of the specific gravity fractions oxidized are shown in table II. Milldale bed coal probably represents, as nearly as it is possible to do so, the "average" coal of the state. The material passing a No. 4 sieve was the only size range oxidized. It was divided into four specific gravity fractions. As in every case the heaviest fraction, which was essentially rock, was discarded. The Black Creek is the most extensive in area of

Jan 1, 1951

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,' there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells' and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported' in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F' (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 '/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By D. H. Thompson, A. W. Tracy

E. A. ANDERSON*—At the outset, I note that you are using a humid atmosphere containing ammonia but that you make no reference to the variable of carbon dioxide content. Edmunds in his work in this laboratory found very marked effects on the rate of failure due to variations in carbon dioxide in the environment. This point is, of course, strongly related to the overall corrosion rate problem since the role of the carbon dioxide seems to be to permit the formation of hygrogroscopic salts which give a controlled moisture film on the specimen surface, which in turn seems to support the intergranular penetration more consistently than would otherwise occur. (2) Your results with various copper binary systems are very striking. It is curious, however, that the time-to-failure minima all occur at percentages of the alloying element which are considerably below the solubility limits as given in the conventional equilibrium diagrams. If your theory regarding the presence of these impurities in some concentration in the grain boundaries is correct, then either the existing diagrams are not accurate in the room temperature region, or there is a difference in solubility in the grain boundaries as compared -with the grains. A study along these lines might be very revealing. (3) The undesirable effect of silicon in copper calls to mind our own observations on the influence of silicon on the stress corrosion cracking resistance of alpha brass. In this case, silicon was found to have a very marked beneficial effect, particularly when a heat treatment capable of producing a grain boundary constituent was used. I should appreciate it if in the discussion of your paper this point should arise, you would attempt to clarify the difference between the copper-silicon binaries and the copper-zinc-sili-con ternary alloys. D. H. THOMPSON and A. W. TRACY (authors' reply)—(1) We have no data on the constancy of the carbon dioxide content of the air used for the test atmosphere but have believed that the normal carbon dioxide content of the air was as constant as could be obtained by using Edmunds' method of removing carbon dioxide from the air and then adding a measured quantity. In any event, the test atmosphere was the same for all specimens in a test run. We agree with Mr. Anderson that the carbon dioxide content is important in the formation of a hygroscopic film on specimens. (2) We can imagine that there could be a concentration of solute atoms at the grain boundaries which would be so small that present methods would not detect it even if it exceeded the solubility limit of the alloy. There could be somewhat greater solubility at the grain boundaries for an interstitial solute. There is a possibility that phosphorus dissolves in this way but we believe that none of the other solutes studied does. In our present studies we hope to find out something about conditions at the grain boundaries of some of the systems mentioned in the paper. (3) Mr. Anderson points out that silicon brass, which has had a high temperature heat treatment followed by a quench. is highly resistant to stress-corrosion cracking. Although the test conditions used by Anderson* et al were different from our test conditions, it is noted that the silicon brasses which had not had the special heat treatment were less resistant to stress-corrosion cracking than copper containing approximately equal amounts of silicon. G. R. GOHN†—Nonferrous metallurgists and particularly, materials engineers, have been accustomed to thinking

Jan 1, 1950

By W. P. Sykes

IN CONNECTION with a study of tungsten steels, Honda and Murakami1 reported an investigation of the system iron-tungsten. This report included a tentative equilibrium diagram, photomicrographs of various alloys in the series, and qualitative measurements of hardness and magnetic properties. The present investigation originally had as its object the study of the hardness and tensile properties of a series of carbon-free iron-tungsten alloys. But, as the work progressed it became evident that the system possessed other features of interest, so the scope of the investigation was enlarged. MATERIALS The iron powder used in preparing the alloys was obtained as follows: Iron oxalate was precipitated from a ferrous-sulfate solution by the addition of a solution of oxalic acid. This oxalate, after thorough washing, was ignited to iron oxide, which after reduction in hydrogen at about 1000° C. yielded iron powder containing but about 0.2 per cent. iron oxide and about 0.005 percent. carbon. Tungsten metal in the form of powder, such as is used in the manufacture of filaments for incandescent lamps, was the other constituent. This material analyzed 99.8 per cent. tungsten and contained no carbon, The metal powders, in the desired proportions, were mixed by tumbling and formed, under pressure of 20 tons per sq. in., into rods 3/8 by 3/8 by 10 in. To form the alloys without contamination, sections of the pressed rods were placed on alundum slabs and heated in an alundum tube wound with a tungsten resistor and packed in heat-insulating material. While the resistor was heated, a stream of hydrogen was continually passed through both the tube and the case containing it. The tungsten winding on the tube, as well as the material heated within the tube, was thus protected from oxidation. Such a furnace will operate constantly

Jan 2, 1926

By L. L. Swift

AT the present time there are four base metals being used for automo-tive bearing alloys. Of course there are numerous variations in the amounts of alloying elements added to each base metal and nearly all of these alloys have the conventional, if not classical duplex structure; that is, they are composed of a hard constituent embedded in a soft matrix. The well-known theory is that the former will wear well, while the latter will be plastic enough to allow the bearing to be broken in and conform to the contours of the shaft. The requirements of the modern bearing have been most aptly described by W. M. Corse: In order to meet the engineering demands of today a good bearing metal must be able to carry the weight of the shaft and stand up under steady or suddenly applied loads, or even blows in some types of service. A certain amount of plasticity is desired to compensate for minute irregularities in the shaft or bearing surface, and to permit yielding, thereby avoiding dangerous stresses in bearing and shaft and pre-venting overheating and rapid wear of parts. Less plasticity is required in a bearing metal if the surfaces of bearings and journals are machined accurately, aligned, and kept in alignment. It is desirable, of course, that a bearing metal have a low coeffi-cient of friction. Under most operating conditions the friction depends on the unit pressure of the bearing, the speed, the temperature, and the properties of the lubricant. A good bearing metal must have a low rate of wear to reduce the necessity for frequent replacements, and adjustment of the bearings. It must wear more rapidly, however, than the journal or shaft running on it, because replacement of the journal or shaft is more difficult and costly than replacement of the bearing.1 The hardness of the bearing alloy is a property closely related to several of the foregoing. With a duplex microstructure, the measure-ment of hardness with any of the usual commercial devices means little. The Bierbaum method of measuring the hardness of the individual constituents was developed to fill this need.

Jan 1, 1938

By Arthur Taggart

THIS paper describes the result of a series of experiments run in the laboratory of the School of Mines, Columbia University, during the winter of 1927-28. It shows that the several operating adjustments of a pneumatic table produce effects in the action of a, given coal that may be grouped into two classes, viz.: stroke length, speed and rocker-arm angle, which affect longitudinal travel; air supply and table slope (transverse and longitudinal), which determine transverse travel. The magnitude of the effect of the different adjustments varies. Some of the adjustments affect stratification of the bed, both as respects size and specific gravity of the bed components, as well as direction of travel. Operation of a pneumatic table is fundamentally different from that of a wet table in that the former exerts, through the air supplied, a force on the particles upward away from the deck which is lacking on the wet table while, on the other hand, it lacks the positive control over cross travel that is supplied by the wash and feed water.

Jan 1, 1929

By C. H. Mathewson

CONSIDERABLE progress has been made during the last few years in analyzing the action of plastic deformation in metallic crystals. This is due largely to the development of X-ray spectrographic methods for studying changes in the orientation of single crystals, or of conglomerates, as they occur during the process of plastic deformation, but partly to the widespread knowledge of suitable technique for preparing large (single or variously combined) crystals for direct crystallographic observation under stress or in various conditions of strain. These two methods of studying changes in the crystalline structure of metals may of course be used in conjunction with features of mutual support, but unfortunately the advantage of direct crystallographic observation is lost when we proceed to the study of severely cold-worked structures, owing to the occurrence of real or apparent crystalline discontinuities which become more and more complicated as the amount of plastic action increases. Furthermore, the X-ray methods do not appear to be adequate, at least in their present stage of development, to fix definitely the character of structural alteration in the parent crystal lattice by plastic deformation. The principal question at issue concerns the nature of the crystalline particles that remain after plastic deformation. These are generally known in our American metallurgical literature as crystalline fragments,1 and they seem, indeed, to diffract as individuals causing the Hull pattern of a, severely cold-worked metal to resemble the pattern of a fine powder,2 with certain features of preferred orientation among the particles determined by the manner and intensity of cold working.

Jan 1, 1927

Jan 1, 1978

By A. I. Krynitzky, Henry S. Rawdon

The most commonly used material for terminals in spark plugs is commercial nickel wire, because of its relatively high temperature of melting, excellent heat conductivity, and slow rate at which the metal is oxidized, even upon continued heating at high temperatures. The grade commonly used for this purpose averages 97 per cent. nickel, the remainder being manganese, cobalt, iron, copper, with traces of other impurities always found in commercial nickel. A peculiar and interesting type of deterioration that occurs in these nickel terminals during the service life of the spark plug was recently brought to the attention of the Bureau of Standards. Commercial spark plugs vary greatly in their size and shape and the terminals differ considerably as to their relative size, shape, number, and arrangement with respect to one another. Although this defect was studied in detail in only one form of spark plug, the deterioration is a characteristic of the material, i.e., of nickel wire, rather than of the particular type of spark plug in which it was noted and studied. The mechanical features of the plugs, however, have a considerable bearing on the time required for the deterioration to become serious. The results of this study of the deterioration of nickel terminals in service should be of value to the makers of all types of spark plugs in which the terminals are made of this metal. CharacteR of Deterioration of WIres During Service Macroscopic Appearance and Properties of Changed Wire.—The nickel terminals in which the deterioration was studied were taken from spark plugs having a central terminal with the ground or side terminals attached firmly at both ends to the shell of the plug. In some of the plugs, two side terminals were used, one on each side of the central one. Although both terminals were found to have deteriorated to some extent, the attack of the central one was quite negligible compared to that of the side ones. These latter wires had developed, in service, transverse cracks that, in many cases, were as sharp and definite as a knife-cut. After a separation occurred, the breach widened by loss of material from the

Jan 1, 1921

By Francis F. Lucas

Jan 1, 1931

By R. B. Woodworth

INTRODUCTION IN the sinking of bore holes, there are but two fundamental operations -drilling and hoisting,-which determine in the main the character of drilling mechanism and structures. There are endless ramifications, however, in the execution of these fundamental operations, according to the purposes for which the bore holes are drilled, their maintenance after completion, the protection and convenience of workmen, etc. The three main lines of use for bore holes are in mineral exploration, the sinking of water and salt wells, and the exploitation of petroleum and natural gas. This paper has to do more especially with the last. Here again there are many divergences. Wells may be drilled by either the percussive, the hydraulic, or the abrasive method. Finally, each of these methods, as applied by drillers of diverse nationalities, has followed somewhat different lines of development. The American system of cable-tool drilling has perhaps had the widest application; the hydraulic rotary is also in extensive use; but the Canadian system, the Galician system, and the Russian free-fall system all have their points of recognized merit and are preferred by operators accustomed to their use. These differences in drilling procedure, which rest ultimately on essential variations in geological conditions, are reflected in the chilling structures as well as in the drilling mechanism. The purpose of the present paper is to record those stages in the development of the application of steel to the construction of drilling mechanism and structures with which the writer has been intimately associated, and to contribute to the history of the art of drilling other data acquired in the course of his personal investigations. It is necessarily limited by reason of space to American practice, with especial reference, therefore, to the cable-tool system and the hydraulic rotary method of drilling wells for oil and gas.

Jan 11, 1915

By M. Kashiwada

The zinc leach residues are introduced into waelz kiln to fume volatile metals and before the end of 1967, the waelz-fume containing zinc, lead, cadmium and indium was directly recycled back to the leaching process for the production of electrolytic slab zinc. However, since 1968, we have been recovering with success those valuable metals contained in the fume separately instead of direct leaching. According to the improved process, the waelz-fume, after being mixed with chloridizing agents, is fed into the rotary kiln to be roasted, wherein most of lead and cadmium content is collected as fume and most of zinc remains in the calcine. Zinc calcine thus obtained, containing 70 to 75 per cent zinc and, less than 1.0 per cent lead is sent to zinc plant for further recovery and the fume containing 40 to 50 per cent lead and 3 to 6 per cent cadmium is further processed to recover lead, cadmium and indium. The advantage of this process can be secured to the utmost when it is combined with the following subsequent treatments. (a) Blast furnace smelting of non-magnetic waelz slag to recover copper, silver and gold as matte. (b) Gallium recovering process from magnetic waelz slag. (c) Soda process of lead bearing cake produced after removing cadmium and indium from the said fume. Thus the extractions of zinc, lead and cadmium from leach residues account for 87 per cent, 72 per cent and 85 per cent respectively.

Jan 1, 1970

By A. M. Gaudin

THIS paper presents, with the help of colored photomicrographs, the new method of mineral identification termed "selective iridescent filming." This method pertains to the field of determinative mineralogy, which it provides with tools for: (1) phase identification, (2) solid solution analysis. The method should be particularly useful in the applied fields of: (1) paragenesis of ore deposits, (2) mineral dressing, (3) mineral synthesis and study of phase equilibria.

Jan 1, 1938