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By Howard Thompson, H. N. Hall, Frank Nuss

Removal of bit cuttings is an important function of drilling muds. In an effort to obtain better understanding of the factors influencing the removal of cuttings, an extensive series of laboratory tests were made in which slip velocities of various sizes and shapes of particles were measured in muds of different physical properties. Empirical equations were then derived from these experimental data. These equations show that slip velocity is dependent on cutting size and shape, mud flow constants, and flow state of the mud. Applicability of these equations for field use is demonstrated by comparing computed slip velocities with slip velocities obtained from field tests. Drilling muds have many functions, but perhaps the most important is the removal of bit cuttings from the well. In a 10,000-ft well, the weight of rock which is drilled and must be carried to the surface is over 150 tons. In addition to this, the mud must remove any sloughings from the well bore. Failure of the mud to promptly remove either bit cuttings or sloughs from the well bore causes re-drilling and excessive wear on bit teeth, slows down drilling rate thereby increasing well costs, and greatly increases possibilities for stuck drill pipe when circulation is stopped for any length of time. Drilling muds lift bit cuttings to the surface by means of the upward velocity of the drilling mud in the annulus. Because a density difference exists between the rock being drilled and the drilling mud, there is a difference between mud velocity and the rate of bit cutting travel, called the net rise velocity. To evaluate the ability of any type of drilling mud in respect to lifting cuttings, some method must be known for predicting the rate of fall of cuttings through mud traveling upwards in the annulus. Equations for the rate of fall of particles through a true fluid have been satisfactorily determined by several authors. 1-6 Since drilling muds are not true fluids, but obey the laws of Bing-ham,7 it should not be expected that equations for rate of fall of cuttings in a true fluid would be applicable to plastic fluids such as drilling muds. Several authors have attempted to compute cutting slip velocities in muds using a viscosity value obtained with a Stormer viscosimeter; however, unsatisfactory results were obtained. Pigott8 took cognizance of the phenomenon of variation of viscosity with velocity in laminar Row, and calculated laminar slip velocities using a variable viscosity with Stokes law, and turbulent slip velocities using Rittingers law. Drilling muds obey the laws of plastic flow which involve factors not affect-

Jan 1, 1950

By L. K. Nemeth, H. T. Kennedy

The investigation presented in this paper was performd to develop a relationship between the dewpoint pressure of a hydrocarbon reservoir fluid and its composition, temperature and characteristics of the heptanes-plus fraction. This is part of an over-all program to develop correlations for the essential properties of reservoir fluids with the composition, temperature and pressure. In all, 579 dewpoint pressures, determined experimentally on 480 different condensate systems along with their compositions and temperatures, were obtained from the literature and from previously unpublished sources. Compositions were expressed in terms of mol fractions of methane through heptanes-plus, nitrogen, carbon dioxide and hydrogen sulfide, and the molecular weight and specific gravity of the heptanes-plus fraction. Distribution of the samples assured a good representation of most of the major oil-producing areas in the world. A multiple regression analysis program written for the IBhl 7094 digital computer was used to compare numerous equations and to calculate their coefficients. The final equation containing 11 coefficients resulted in an average absolute deviation of 7.4 percent for all the samples. Segregation of data on the basis of one or more variables did not materially improve the results. The correlation developed is useful in predicting the dewpoint pressure of condensate reservoir fluids from variables normally measured in the laboratory. INTRODUCTION In any discussion of the dewpoint of hydrocarbon mixtures, it should be noted that there are two kinds of dewpoints which must be distinguished. The first type, or normal dewpoint, usually occurs at low pressures as dry gas is compressed to the point where liquid first forms. The second type, sometimes called the retrograde dewpoint, occurs when a gas mixture containing heavy hydrocarbons in solution is depressured until a liquid is formed. The first type, as applied to condensate mixtures, would normally be below atmospheric pressure and would be of no interest in reservoir performance. The second type is of great significance in interpreting reservoir behavior and is the property referred to throughout this paper. Laboratory measurement of dewpoints is laborious, expensive and subject to many errors, and it is desirable to find a reasonably accurate method to predict dewpoint pressures from the composition and other readily available properties normally measured on the fluids. A possible method of calculating dewpoint pressures would be to employ a set of equilibrium ratios (K-values). 1 However, the K-values themselves depend on composition as well as temperature and pressure; presently their use adds nothing to the accuracy of predicting dewpoints. If future correlations provide a significantly better method of estimating K-values for heavy hydrocarbons, they may be of greater use. REVIEW OF LITERATURE In 1944, Olds, Sage and Lacey 2 studied the behavior of fluids from the Paloma field. Properties of seven mixtures were studied at temperatures ranging from 100 to 250 F and at pressures up to 5,000 psia. From the information obtained, the influence of composition and temperature upon the dewpoint was determined. It was found that removal of the intermediate molecular weight components from the mixture resulted in considerable increases in the dewpoint pressures. Results indicated that the effect of changes in temperature was relatively minor when compared with the effect of modifying the mixture by removing the intermediate components. Thus, removal of propane and butanes resulted in an increase in dewpoint pressure more than 10 times greater than a change in temperature from 100 to 250 F. The authors stated that althouah

By W. A. Backofen, G. Mayer

Single crystals of iron, copper, and a Cu-7 wt pct A1 alloy were pulled through conical dies to simulate the constraint in a polycrystalline aggregate undergoing axisymmetric reduction. With Taylor-type hardening, dependence of the drawing stress, od, on the Taylor orientation factor, M, is predictable from the polycrystal stress-strain curve; in particular, for a power-law relationship, it should follow that d log od/d log M = (1 + n). A first-order agreement with analysis was found in the data from iron. For copper, the implied n from the observed d log od/d l°g M was -0, while for Cu-7Al it was negative. The trend was in the direction of random polycrystal behavior. Thus the idea of hardening only in response to the amount of prior slip loses validity as stacking fault energy (SFE) is lowered. Two possible explanations have been suggested: as stacking fault ribbons are widened, barriers from dislocation reactions become increasingly effective in dispersing slip and reducing the orientation dependence of the total glide strain dm that appears in alternatively, or conjointly, the polyslip shear stress, 7, acquires an orientation dependence of a kind which has the same leveling effect on M. The problem of relating the strain hardening of polycrystalline material to that of an isolated single crystal is still largely unsolved. In a new experimental approach from recent work, single crystals of different orientations have been deformed under the constraints found in an aggregate while measuring their deformation resistance. Procedures have involved drawing cylindrical crystals through conical dies1 and compressing slab-shaped crystals in plane strain.2'3 Predictions for the outcome of such experiments were made first by Taylor~ and later, in more general form, by Bishop and Hill.5'6 Taylor's example was the axisymmetric extension of an fcc crystal slipping on the usual {111}(110) systems or, equivalently, a bcc crystal undergoing 'kestricted" slip on {110}(111). In his solution, the deformation work supplied was equated to that dissipated internally in slip on all active systems. With o the single applied tensile stress, dc the resulting axial strain, and dyT the total glide strain on systems operating at resolved shear stress, 7: The orientation dependence of M was found by minimizing dyT for each orientation while activating five independent systems, Fig. l(a).? The Bishop and Hill analysis, based on a principle of maximum work, leads to essentially the same conclusion; the need for at least five active systems is recognized in the finding that either six or eight are actually brought into operation. The mean value from the entire stereo-graphic triangle in either case is M - 3.06. More recently, Hutchinson8 made a Taylor-type analysis for pencil glide in a bcc structure, from which piehlerg prepared Fig. l(b) as the counterpart in Fig. l(a); here M = 2.75. The obvious weakness in such analyses is the indifference to slip-system interactions. A condition of what might be termed "independent"

Jan 1, 1969

By D. J. Carney, E. C. Rudolphy

Large macroscopic nonmetallic inclusions were related to altered fireclay refractories by chemical and microscopic means. Pouring refractories are discussed as a source of these large inclusions. Nozzles and wells are major contributors. Use of alkali and titania contents as tracers is described. Recommendations are offered to minimize the sources of inclusions from pouring refractories. IN any attempt to improve the cleanliness of plain carbon and alloy steels, consideration must be given not only to the proper deoxidation practice to minimize inclusions, but also to sources of inclusions from pouring refractories. In some cases, the inclusions resulting from deoxidation may be minor in amount, yet a relatively dirty steel may be produced as a result of improper care in the pouring practices for the steel. The number of studies of inclusions resulting from pouring refractories has increased recently and some excellent reports on this subject have already been published.'4 Some of these reports were reviewed briefly in a companion paper by M. P. Fedock.5 Mr. Fedock's contribution is a fine addition to the studies necessary to improve steel cleanliness for the ultimate benefit of all steel producers and consumers. In the interest of constantly improving cleanliness, the authors have been actively engaged for the past two years in experimentation to determine more closely the sources of inclusions in steel. One phase of this work was associated with efforts to define more closely the sources of macroscopic inclusions which have been experienced on occasional heats. The term "macroscopic inclusions" is defined in general as those inclusions which are visible to the naked eye or at low magnifications of the order of less than X25. These inclusions sometimes can be seen in the macro-etch tests of billets and slabs. This report summarizes a few of the field experiments and laboratory studies conducted at the South Works of the United States Steel Corp., which were made regarding nozzles, wells, and ingot scums, as well as inclusions occurring in steel products. The data in the present study, together with the data of Mr. Fedock concerning ladle erosion, should be of value in regard to future studies of inclusions arising from pouring refractories. The knowledge gained as a result of data collected thus far at South Works has been helpful in improving the cleanliness of the products and in pointing the way toward further improvements. Similarity of Large Inclusions to Refractories and Altered Refractories In the routine inspection of billet etch tests, occasional inclusions visible to the naked eye have been observed. These large inclusions most frequently occur near the top of the ingot and near the billet surface. When such material was encountered, careful examinations were made in an attempt to determine the origin of these inclusions. In a relatively few cases, examination revealed that the material was unaltered fireclay refractory of a type similar to that used for hot-top material, with only the surface of the inclusions having an altered appearance under the microscope. However, the great majority of these inclusions were completely altered-refractory material. The term "altered refractory" is defined

Jan 1, 1955

By L. A. Bromley, R. L. McKisson

A high temperature calorimeter designed for use up to 1500°K is described and the theory of its operation presented. This calorimeter was used to measure the heats of formation of Na-Sn alloys ranging in composition from tin to Na2Sn. The values tend to support those reported by Kubaschewski and Seith. ONE method of obtaining the heat of formation of an alloy is to measure the heat of mixing of the elements at high temperature. The principal advantage of this method is that the desired quantity is measured directly, while in conventional room temperature methods the differences of the heats of solution of the elements and the alloy in a suitable solvent are measured. A method of improving the accuracy of the high temperature measurements, when the precision of the measurement is lower than that of the heat capacity values for the elements, is to add one component at room temperature to the other at the high temperature, so that part of the heat of reaction is dissipated in heating the cold component to the high temperature. Thus, only a fraction of the heat of reaction is measured, and a result of higher precision is obtained. The limitations of the high temperature technique are that volatile systems cannot be studied, and that many alloys melt at temperatures higher than those at which the calorimetric apparatus operates readily. Nevertheless, a calorimeter operating at 1500°K would be useful in investigating many of the lower melting alloy systems and the low melting mixed oxide systems. A unit designed for these applications was built and is described here. The Na-Sn system was chosen for investigation because the temperature involved, 880°K, would adequately test the operation of the calorimeter. Further, the data reported in the literature for the various alloys of sodium and tin differ markedly, and it was hoped that this investigation would help to fix the values of the heats of formation in this system. Design of Apparatus A detailed discussion of the considerations involved in the calorimeter design is given by Mc-Kisson and Bromley,' and a brief summary follows. Fig. 1 shows a sectional view of the calorimeter. The inner graphite chamber is maintained at constant temperature by means of the circulating molten tin bath in which it is submerged. The tin is contained in a graphite vat. This unit comprises a thermostat whose heat capacity is about 7000 cal per "C. The main heating element consists of a machined graphite spiral with a room temperature resistance of about 1/2 ohm. These parts are separated from the powdered carbon external insulation by the cage, a cylindrical graphite chamber. The electrical insulators and separators, the auxiliary heater spool, and the loading tube liner are made of sintered alumina. The tin vat stirrers, the sample stir-rer, the melt thermocouple well, and the power leads are made of molybdenum. The auxiliary heater is wound with molybdenum wire and serves to compensate for the heat loss up the loading tube. All of the individual components in the high temperature region of the calorimeter will withstand at least 2000°K, and the various contacting materials should easily withstand 1500°K. The external container for the insulating carbon powder is a copper shell upon which copper tubes are soldered to serve as cooling coils.

Jan 1, 1953

By L. O. Bacon, D. O. Wyble

THERE has been considerable speculation among mining geologists and mining men in general as to the relative merits of gravity methods in iron-ore exploration. Most of the investigations which have been carried out in recent years have been done by mining companies, and few if any of the results have been published. Three gravity surveys have been made in the Iron River-Crystal Falls area,1,2 one by the U. S. Bureau of Mines, with inconclusive results, and the other two by Radar Exploration Co. for the Cleveland-Cliffs and the M. A. Hanna companies, with results not known to the writers. Both the last-mentioned surveys were detailed investigations, the stations being spaced as close as 10 ft along traverses,1 and were made to determine the feasibility of locating iron ore by gravitational methods. Because of the presence of a large body of ore already extensively drilled, Dr. Harold L. James of the U. S. Geological Survey, Iron River, Mich., suggested that a further test of gravitational methods of exploration be made in the Round Lake area of Iron County, see Figs. 1 and 2. This survey indicated a considerable regional gradient and led to a study of the surrounding gravity field and its relation to the major structural features of the syncline within which the iron formation lies. The southwestern part of Iron County presents a series of hills and hollows elongated in a roughly north-south direction. The bedrock topography is of pre-glacial origin. Relief is moderate; a maximum elevation difference of approximately 350 ft was observed during the survey. Major drainage is dendritic with the larger streams: the Brule to the south, the Paint to the north, and the Iron in the central part. Hills are thickly grown with hardwoods, and lowland areas, not under cultivation, are usually covered by second-growth softwoods. The area covered in this paper includes the southern half of Iron County, Mich., with a deep synclinal basin occupying the central part of the area, and the southeast corner of Gogebic County, immediately to the west of Iron County. The upper Huronian iron formation, slates, and graywackes which form the synclinal basin rest upon a greenstone basement. The basin has not been completely outlined by exposures, drill records or other means, as outcrops are scarce and the thick mantle of glacial drift makes geological investigations extremely difficult. Glacial drift varies in depth up to 300 ft or more. The drift is usually thickest under the hills and is thinnest in the depressions and along drainage courses where most of the bedrock exposures occur. The area over which gravity investigations were made is almost entirely covered by glacial material. Bedrock of the basin consists of a complexly folded series of iron formation, slates, and graywackes. One of the series of slates has a high magnetic susceptibility due to the fine-grained magnetite it contains. This formation can be detected readily by magnetic methods and provides a marker horizon which can be easily followed. The magnetic slates are stratigraphically above the iron formation, and much of the geological interpretation of the area is based upon the magneticc anomalies they produce.

Jan 1, 1952

By Howard R. Keil

Reactor at Carlton mill successfully calcines pyrite-telluride flotation concentrate for cyanidation. CARLTON mill in the Cripple Creek district, 45 miles southwest of Colorado Springs, Colo., has been in operation for approximately three years, treating the custom sulpho-telluride ores formerly handled by the Golden Cycle mill in Colorado Springs. At the new mill the pyrite-telluride flotation concentrates have been roasted, prior to cyani-dation, in a Dorrco FluoSolids reactor, which has proved capable of yielding calcine readily amenable to cyanidation. Incoming ores are crushed at Carlton to % in. and sampled in 30 to 75-ton lots before the individual lots are mixed in the fine ore bin. The composite ore then goes to the grinding circuit. Classifier overflow from the grinding circuit is treated by flotation to produce a concentrate containing approximately 85 pct of the values in 5 pct of the weight. The flotation concentrate goes to the FluoSolids reactor prior to cyanidation. Cyanide solution values are recovered by zinc dust precipitation. Flotation tailings are thickened and cyanided, the values from this part of the circuit being recovered from solution by activated carbon. Gold values in the flotation concentrates consist of a small amount of finely divided metallic gold; the tellurides, sylvanite and calaverite; and gold very intimately associated with the pyrite. The metallic gold and a part of the telluride values can be extracted from the concentrates by cyaniding without roasting. However, extraction on the tellurides by this method is not satisfactory, and the pyrite values are so intimately associated with the pyrite that very fine grinding and cyanidation for a prolonged period under ideal laboratory conditions does not yield good recovery. Upon roasting, the tellurides are oxidized to very finely divided metallic gold which is readily soluble in cyanide. The pyrite is oxidized mainly to a porous iron oxide which allows cyanide solution to penetrate to gold particles and take them into solution. Feeding the Reactor Flotation concentrates move by gravity to a thickener. Thickener underflow is discharged at approximately 60 pct solids, by means of a diaphragm pump, into a storage and blending agitator. From here the concentrates are pumped to a disc filter. The filter cake, at 84 to 88 pct solids, drops directly into a repulper where it is repulped into a slurry of 78 to 80 pct solids. The repulped filter cake flows into a 6x6-ft slurry agitator from which it is fed directly into the reactor by the Moyno pump. The Moyno pump has eliminated a large number of difficulties that were first encountered in feeding a wet concentrate to the reactor. On the original installation in Canada a screw feeder was used to introduce the filter cake directly into the reactor. Since the reactor is under a slight positive pressure it was necessary to have a suitable seal to prevent gas escaping from the reactor at this point. When the concentrates produced in flotation were coarse or granular they could be readily fed to the reactor but when fine-textured, clayey concentrates were produced a great deal of trouble was encountered.

Jan 1, 1955

By A. V. Deforest, C. W. Macgregor, A. R. Anderson

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942

By H. J. R. Way

The work to be described was undertaken at various periods from 1937 to 1939 on the Busia gold field, in the eastern province of Uganda. It was decided to examine the possibility of reef prospection by the resistivity method, for it was not known how far the usually disintegrated nature of most reefs in the ubiquitous laterite near the surface would obscure indications obtained by resistivity traverses. The work at the commencement was therefore largely experimental, but the results obtained thereby were satisfactory, and a survey was started at the Government closed area at Amonikakine. With the limited time and resources at the writer's disposal, it was not possible to complete the survey to his satisfaction or to follow up exhaustively all the geophysical indications, but some of the results of the experimental work and the survey were of sufficient interest to be worth recording; in particular the relation between the width of reef, electrode separation and shape of the curve, and the interference effect of constant separation curves over zones of float are significant and useful. Three new veins were located, but only one contained sufficient gold to warrant detailed prospection. This was called the Geophysical reef, and was uncovered over a strike distance of 1140 ft., and there are indications that it extends over a distance of 1990 ft. These results and the recom- mendations consequent therefrom were embodied in a special report to the Uganda Geological Survey. History OF the Field The Busia field is in the southeastern corner of Uganda near the Kenya-Uganda border, and is about 17 miles north of the northeastern corner of Lake Victoria. Gold was first discovered in the area in the stream beds by Davies1,2 in 1932. Subsequently numerous small alluvial claims were worked by prospectors and the area was prospected for reef by a company for periods varying from three to nine months, but was finally abandoned, as the results were considered unfavorable. Further prospecting by the Geological Survey in 1935-1936 under Davies8 and later under the writer4 uncovered three reefs with sufficient gold values to be of economic interest. These were finally taken over by a company known as Borderland Syndicate, which still owns the area, and from September 1937 to the end of 1941 about 13,000 oz. of gold was extracted from reefs of the area proved by the Geological Survey. Opencast mining operations are still proceeding (February 1943). The Amonikakine area lies to the immediate north of that of Borderland Syndicate. A certain amount of prospecting had been done when the writer started work there. As a result of his report, this area was taken over by another syndicate, but little further work was accomplished before it ceased operating because of difficulties of wartime working.

Jan 1, 1946

By Charles C. Towle, Irving Rapaport

URANIUM mineralization along the north flank of the Zuni Uplift, in the vicinity of Haystack Butte, was discovered by Paddy Martinez, a Navajo Indian, in the spring of 1950. The find was reported to the Santa Fe Railway Co., which initiated a program of exploration upon its holdings in the district in December of 1950. The Anaconda Copper Mining Co. secured numerous leases in January and February, 1951, and began an intensive exploration and development program in March 1951. The district was extended into the Lucero Uplift in August of 1951 by the discovery of uranium mineralization in Todilto limestone by Joy Sinyella, a Supai Indian living on the Laguna Reservation. Initial reconnaissance was performed in the district by the Atomic Energy Commission in November 1950. A field office under the direction of the Denver Exploration Branch of the AEC was established at Prewitt, N. Mex. in January 1951 to study regional and detailed guides to ore, to evaluate the ore deposits, and to promote the development of the district by providing geologic services for the companies and individuals engaged in exploration. With the development of sufficient ore to warrant construction of a mill, the Grants area of New Mexico has come of age as a full fledged uranium mining district. The carnotite-type deposits of Grants, the first of major economic importance found in limestone, have extended the Colorado Plateau carnotite field into the more complex structure of the Basin and Range Province. General Geology The Grants uranium district is in northwestern New Mexico, along the southern flank of the San Juan Basin, between the cities of Gallup and Albuquerque. The region is at a mean altitude of about 6800 ft, vegetation is sparse, and outcrops are excellent. Mt. Taylor volcanic peak, at an elevation of 11,400 ft dominates the surrounding area. The overlying cliff-forming Dakota sandstone is the most resistant formation in the Grants District and characteristically erodes into dissected mesas as much as five miles wide. The principle uranium ore-bearing horizons are found in the underlying Morrison formation, and the Todilto limestone of the San Rafael group. The Morrison weathers into. a series of steep slopes and precipitous cliffs near the lower part of the Dakota-capped rims, while in contrast, the relatively resistant underlying. Todilto [ ] limestone forms broad benches extending out from the base of these Dakota rims as much as five miles wide. The Todilto benches are covered with overburden to an average depth of about 5 ft in the first thousand ft away from the Dakota rim, but increases to about 200 ft at the base of the rim. In many places however, a thick mantle of upper Cretaceous sediments and Tertiary volcanics "obscures the ore-bearing Jurassic, and precludes exploration. . The known uranium deposits of the Grants District are distributed throughout a zone 85 miles long and about 10 miles wide. Stratigraphy Rocks from pre-Cambrian through Tertiary are exposed in the uplifted areas, but uranium appears to be restricted chiefly to two zones in Jurassic sediments. The Jurassic sediments of the Colorado Plateau have been subdivided into three units, in ascending order: (1) Glen Canyon group, (2) San Rafael group, (3) Morrison formation. The Todilto limestone zone within the San Rafael group has produced the bulk of ore to date, but the promise of the Morrison zone is rapidly increasing. The Todilto formation extends about 300 miles east-west and about 100 miles in a north-south direction. It is composed of a lower, extensive, limestone member and a central, more restricted, thick, pure gypsum member. The Todilto is believed to be of lacustrine origin. The Morrison formation in this area is subdivided, rather arbitrarily, into three members: Recapture Creek, Westwater Canyon, and Brushy Basin. Ore

Jan 1, 1952

By A. V. Deforest, A. R. Anderson, C. W. MacGregor

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942

By H. Warlimont

Precipitation of cementite plates from carbon-rich austenite gives rise to localized formation of martensite in the matrix next to the precipitate upon quenching. The growth of this martensite is urmsually restricted. A distinct lattice relationship is found between this martensite and the cementite phase. It is concluded that the martensite is nacleated in the region of lowest carbon concentration at the austenite-cementite integace, with low-energy matching to the cementite lattice. The restriction of the growth of the martensite phase to the vicinity of the cementite plates can be explained by misfit in the austenite -martensite glissile interface and the uphill carbon gradient in the austenite. The investigation was carried out by light- and electron-microscopy and by electron-diffraction of thin foils. THE precipitation of cementite from carbon-rich austenite gives rise to a localized formation of martensite in the matrix next to the precipitate upon quenching. This behavior has been described previously by A. B. Greninger and A. R. Troiano1 for a 1.78 pct C steel ("pseudomorphic martensite"), and by A. Hultgren2 for a Fe-0.99 pct C—5.20 pct Mn steel. By measuring the axial ratio of the martensite phase,' it was found that the carbon content of this martensite was lower than that of the martensite which formed without prior partial transformation to cementite. Therefore, it was concluded that lowering of the carbon concentration in the matrix next to the precipitate raised the M, temperature locally and thus led to nucleation of martensite at the ce-mentite-austenite interface. However, the restriction of the growth of the martensite phase to the vicinity of the cementite plates cannot be explained by localized carbon impoverishment alone. Under ordinary conditions a martensite plate which has been nucleated in a favorable site can continue to grow until it encounters a physical barrier, or until it encounters a compositional barrier in the matrix, where the total free-energy change for the reaction is not negative, since it has been shown by numerous experiments that the activation energy for growth of ordinary martensite is virtually zero.' An investigation was conducted by transmission electron microscopy and electron diffraction to study this extraordinary martensite. It was expected that crystallographic in addition to compo- sitional conditions caused this abnormal mode of martensite formation. MATERIAL AND PROCEDURE An Fe-C-Mn alloy containing 1.15 pct C and 5.1 pct Mn was used for most of the experiments. For metallographic work, specimens 15 by 15 by 3 mm were used. For preparation of thin films, the initial specimen size was 15 by 15 by 0.7 mm. The heat treatment of each specimen consisted of austenitizing for 1/2hr at 1100'~ in an argon atmosphere, subsequent isothermal holding in a lead bath at one of a series of different temperatures, and, finally, quenching into brine at room temperature. For metallographic examination, the specimens were mounted in bakelite (slight tempering effects resulted from the heat in the mounting press) ground, polished, and etched in nital. Thin films for transmission electron microscopy and electron diffraction were obtained by grinding the specimens to approximately 0.2 mm thickness and subsequent electrolytical thinning. The orientation relationships were evaluated from sets of electron micrographs and selected-area electron diffraction patterns of single units of the transformation products and the adjacent matrix. RESULTS In the alloy which was used for the experiments, proeutectoid carbide precipitates over a wide tem-

Jan 1, 1962

By H. J. R. Way

The work to be described was undertaken at various periods from 1937 to 1939 on the Busia gold field, in the eastern province of Uganda. It was decided to examine the possibility of reef prospection by the resistivity method, for it was not known how far the usually disintegrated nature of most reefs in the ubiquitous laterite near the surface would obscure indications obtained by resistivity traverses. The work at the commencement was therefore largely experimental, but the results obtained thereby were satisfactory, and a survey was started at the Government closed area at Amonikakine. With the limited time and resources at the writer's disposal, it was not possible to complete the survey to his satisfaction or to follow up exhaustively all the geophysical indications, but some of the results of the experimental work and the survey were of sufficient interest to be worth recording; in particular the relation between the width of reef, electrode separation and shape of the curve, and the interference effect of constant separation curves over zones of float are significant and useful. Three new veins were located, but only one contained sufficient gold to warrant detailed prospection. This was called the Geophysical reef, and was uncovered over a strike distance of 1140 ft., and there are indications that it extends over a distance of 1990 ft. These results and the recom- mendations consequent therefrom were embodied in a special report to the Uganda Geological Survey. History OF the Field The Busia field is in the southeastern corner of Uganda near the Kenya-Uganda border, and is about 17 miles north of the northeastern corner of Lake Victoria. Gold was first discovered in the area in the stream beds by Davies1,2 in 1932. Subsequently numerous small alluvial claims were worked by prospectors and the area was prospected for reef by a company for periods varying from three to nine months, but was finally abandoned, as the results were considered unfavorable. Further prospecting by the Geological Survey in 1935-1936 under Davies8 and later under the writer4 uncovered three reefs with sufficient gold values to be of economic interest. These were finally taken over by a company known as Borderland Syndicate, which still owns the area, and from September 1937 to the end of 1941 about 13,000 oz. of gold was extracted from reefs of the area proved by the Geological Survey. Opencast mining operations are still proceeding (February 1943). The Amonikakine area lies to the immediate north of that of Borderland Syndicate. A certain amount of prospecting had been done when the writer started work there. As a result of his report, this area was taken over by another syndicate, but little further work was accomplished before it ceased operating because of difficulties of wartime working.

Jan 1, 1946

By C. H. Li, S. H. Bendel, J. A. Sartell

Small additions of Mg to a 62 Cu-38 Ni alloy reduce the oxidation yates drastically between 500° and 850°C. Metallographic examination of the oxide scale disclosed a continuous network, identified by X-ray diffraction as (Ni, Mg)O solid solutions, located along the former alloy grain boundaries. This network acts as a barrier to diffusion. It is thought to result from the segregation of mg to the alloy grain boundaries. Oxidation occurs preferentially in these regions because of the presence of this more active element. To substantiate these ideas, homogenized alloys ulere oxidized. No oxide network was produced and oxidation rates were the same as for the parent 62 Cu-38 Ni alloy. An interesting aspect of the oxidation of the 62 Cu-38 Ni alloy previously described by the present authors, is the relationship between oxidation kinetics and changes in the microstructure of the oxide.' The oxide scale on these alloys consists of two layers: a thin layer of CuO outside a much thicker layer of Cu20 in which particles of NiO are dispersed. In addition, immediately beneath the oxide-metal interface there is an internally oxidized zone in which NiO particles are dispersed in a copper-rich alloy matrix. Experimental observations on the growth of the individual layers under isothermal conditions have led to the conclusion that the rate-determining step in the oxidation of this alloy is the diffusion of anions through the Cu20 layer. It has been found that this diffusion rate is increased by the recrystallization of the outer CuO layer. Willardson and Gorton have reported that the addition of magnesium to the 62 Cu-38 Ni alloy causes a decrease in the oxidation rate.2 The present investigation was undertaken in order to determine the mechanism by which magnesium additions improve the oxidation resistance of the 62 Cu-38 Ni alloy. EXPERIMENTAL PROCEDURE Fifty-gram ingots of Cu-Ni alloys were prepared by vacuum melting materials of 99.999+ pct purity. These ingots were then remelted in a He atmos- phere and magnesium added in the form of a previously prepared and analyzed Cu-Mg master alloy. This procedure was necessitated by the high reactivity of pure magnesium at high temperatures. The proportion of the alloying elements was adjusted so as to obtain alloys with the desired magnesium content while maintaining a Cu-Ni ratio of 62 :38 by weight. (All alloy compositions will be given in weight percent.) Since it was considered desirable to study the oxidation of only single-phase, solid-solution alloys, it was necessary first to determine the approximate limit of solid solubility of magnesium in the 62 Cu-38 Ni alloy. A series of melts with various magnesium contents was made, homogenized by annealing for 48 hr at 975OC, then cooled in the furnace. Metallographic samples were prepared, etched in a potassium dichromate solution and examined at XI500 for the presence of a second phase. The alloys were then chemically analyzed and it was found that the approximate limit of solid solubility of magnesium in the 62 Cu-38 Ni alloy was 1 pct Mg. The ingots containing less than 1 pct Mg (0.19, 0.29, 0.58, and 0.87 pct Mg) were cold-rolled down to thicknesses suitable for oxidation experiments and specimens for gravimetric studies were cut to dimensions of 3.0 by 1.5 by 0.05 cm, specimens for inert marker studies, 0.6 by 0.6 by 0.17 cm. These were heat-treated in a protective atmosphere at a temperature (975" C) well above the oxidation temperatures and furnace-cooled to insure structural stability of the alloy during oxidation. Immediately prior to oxidation, the specimens were chemically cleaned by immersion for 1 min in a solution of 2 parts nitric acid, 1 part acetic

Jan 1, 1961

By H. R. Brannon, R. J. Robinson, G. W. Kattawar

Accurate prediction of storm wave characteristics are needed for design of offshore structures. Statistical methods of random noise analysis provide techniques for predicting required wave properties. These techniques have been used to analyze and characterize storm wave profiles from Gulf of Mexico recording installations in 34, 65 and .98 ft of water. Correlations based on the results can be used to predict wave crest probabilities and wave shapes for a range of Gulf water depths and storm conditions. Example predictions of wave crest probability as a function of water depth for a particular set of storm conditions are given. INTRODUCTION Accurate predictions of wave crests and wave shapes are needed for design of offshore structures. With predictions of wave crests, platform deck elevations giving adequate protection from exposure to storm waves can be selected. Use of hydro-dynamic wave theories with the wave crest and wave shape predictions permits an estimate of the wave forces an offshore structure must withstand. Observation of ocean waves suggests use of statistical analysis for studying wave characteristics for water depths beyond the breaking wave zone; recent wave generation theories lend support to this approach. l-3 One of the most powerful methods of statistically analyzing wave profiles was introduced by Cartwright and Longuet-Higgins; most of the basic relations used were developed by Rice5.6 in studies of random noise theory. This method predicts wave crest elevation probabilities from two parameters characterizing a wave profile. The statistical approach also provides a means for predicting wave shapes. In the random noise model of a wave profile, surface elevation is represented as an infinite sum of sine waves with closely spaced frequencies and random phase angles. Power density is proportional to the sum of the squares of the amplitudes of sine waves having frequencies within a narrow band, and the distribution of power density as a function of frequency is called the power density spectrum, or power spectrum. The power spectrum characterizes an irregular sea, and hence finds use in motion studies of ships, barges and semisubmersible drilling platforms. From the power spectrum, a wave profile of any duration of time can, in principle, be calculated; this long wave profile depicts the many wave shapes to which a structure may be exposed. Thus, the statistical methods of wave analysis provide an approach to selecting wave shapes as well as wave crest elevations needed for design of offshore structures. For practical application of these techniques, power spectra and related quantities must be predicted from storm properties. Barber and Tucker 7 have reviewed correlations of wave properties and storm conditions. Their review summarizes work of Darbyshire,8 among others, in which a correlation of power spectra with wind intensity of the North Atlantic was developed. These results, plus more recent work by Pierson and Moskowitz and Kitaigorodskii,10 establish feasibility of correlation, but there is no theoretical basis for modifications extending the relations to other areas as remote as the Gulf of Mexico. Hence, to predict characteristics of Gulf of Mexico waves, a study of local observations is needed. This paper presents (1) a practical approach to computing wave profiles hat depict shapes of waves for use in force calculations, (2) a summary of relations for predicting probabilities of wave crest elevations, (3) correlations of parameters needed to apply these methods in the Gulf of Mexico and (4) examples of application of the techniques. THEORETICAL BACKGROUND The following sections summarize relations needed to calculate wave profiles and to estimate wave crest probabilities. These relations also identify quantities that must be related to storm

By G. G. Priest, B. E. Morgan

The production of oil and gas from wells is often seriously hindered by the compaction of solids in the perforations during the perforating process. To realize the full productive capacity of a well, it is necessary either to remove the plugging material from the perforations or to perforate in a manner which does not cause plugging of the perforations. The latter method can be accomplished by having a non-plugging fluid in the casing at the time the well is perforated. This paper describes the results of laboratory tests, perforating tests, and experimental field tests which demonstrate that certain emulsions serve effectively as non-plugging perforating fluids. The principal components of these emulsions are two liquids: an aqueous phase consisting of a solution of either sodium chloride or calcium chloride, and an oil phase consisting of diesel oil, tetrachloroethylene, or a combination of both. Small amounts of other agents which serve to stubilize the emulsions, to reduce the fluid loss, and to inhibit corrosion are also present. The density of the emulsions is controllable within the range of 7.5 to 12.5 lb/gal; no insoluble solids are present, the filtration rate is low, and the thermal stability is satisfactory at temperatures as high as 200°F. The corrosion of steel by these emulsions is negligible. Tests conducted under conditions which simulate the temperature and the pressure in an actual well demonstrate that these emulsions fulfill the requirements of a non-plugging perforating fluid. In addition, lirnited field experience furnishes evidence that these emulsions remain in position after they are spotted, that they are retained in the casing after the perforations are made, and that they are easily removed from the perforations when the well is opened for production. When the pressure in the borehole is greater than the formation pressure at the time a well is perforated, plugging of the perforations can be avoided by spotting an emulsion adjacent the interval to be perforated. This procedure should eliminate low well productivity caused by plugging the perforations. INTRODUCTION Nature of Problem The most widely used method for the completion of oil and gas wells is to set and cement casing through productive horizons, and then to obtain production by gun-perforating the section of casing opposite the desired interval. This method is gen- erally successful and it was thought at one time that those failures which did occur were due to insufficient penetration by the perforator. Despite recent improvements in perforators which assure ample penetration, unsatisfactory fluid production continues to be a problem. Evidently, the trouble comes from some other source. Recent results obtained by Allen and Worzel1 demonstrated that low fluid productivity may be caused by the perforating process and/or by the fluid in the wellbore at the time of shooting. They found that perforations are often completely plugged by debris from the perforator, pulverized sand from the formation, and compacted solids from the drilling mud when the pressure in the wellbore is greater than the pressure in the formation at the time of perforation. In some cases a differential pressure in excess of 400 psi was required to initiate flow into the well through these plugged perforations. The plugging of perforations by solids not only causes low productivity from wells, but it creates simultaneously other problems in the production of oil and gas. For example, when most of the perforations are plugged, high rates of flow must occur through the few perforations that are open. The resulting high pressure drop may cause production

Jan 1, 1958

By R. A. Morse, C. R. Holmgren

The production of oil by water flooding can be substantially increased by the maintenance of free gas saturation in the reservoir during the flooding operation. This effect is accomplished by the alteration of oil relative permeability characteristics and the occupation by gas of pore space that would otherwise be filled with residual oil. The amount of reduction In residual oil can be calculated from appropriate water-oil relative permeability characteristics. This paper presents experimental data in support of the foregoing conclusions and an example of the calculations. The microscopic pore saturation concepts of the mechanism are discussed. A method of practical application to field floods is presented together with discussion of certain limitations. INTRODUCTION The presence of free gas has been reported by a number of investigators to significantly affect the oil recovery which can be obtained from sandstone flow systems by water flooding.1,2,3,4,5 The effect of gas, noted in every instance, has been to cause lower residual oil saturations than could be obtained by water flooding the same systems in the absence of free gas. The degree of improvement in recovery has been observed to vary widely, depending on the systems used and the conditions of the tests. The increased oil recovery obtained because of the presence of gas during a water flood has been variously attributed to changes in physical characteristics of the oil, selective plugging action of the gas, inclusion of oil mist in the free gas phase, and the additional sweeping or driving action of the free gas. All but the first of these suggestions imply changes in the displacement mechanism. The change in viscosity and inter-facial tension of the oil phase, within the pressure range used for all the experimental work, is certainly not sufficient to account for the differences in residual oil saturation noted dess there is a drastic change in the displacement process. One other effect which logically seems capable of causing differences in residual oil saturation of the magnitude noted in the experimental work is that of simple replacement. In a water-wet system containing oil, water, and gas, it is to be expected that the gas will exist inside the oil. This is the position of minimum free surface energy, since the gas-oil interfacial tension will be less than the gas-water interfacial tension. There is no apparent reason to expect that the existence of free gas within the oil phase should alter the saturation at which the non-wetting phase (now oil and gas) should become discontinuous and hence trapped so as to be unrecoverable by direct displacement by water. If this is the situation, then trapping of a certain percentage of gas saturation during water flood should result, at infinite water-oil ratio, in a like reduction of oil saturation below that attainable by flooding in the absence of free gas. It is visualized that the gas will exist as bubbles inside the discontinuous residual oil as illustrated in Fig. 1, with the size of the oil bubbles being substantially unchanged due to the presence of the gas. As a practical matter, it can be anticipated that the presence of a free gas saturation inside the oil phase will reduce the relative permeability to oil which will exist at any particular water saturation. This reduction will be caused by two factors — -the addition of the gas-oil interface, and the reduction of area available for oil flow in the pores containing gas. This reduction in oil permeability at any particular water saturation will result in water breakthrough at a lower water satu-

Jan 1, 1951

By P. R. Swann, J. G. Parr

Quenched structures were studied in alloys containing up to 12.5 pct cobalt. The subsequent decomposition of a 10 pct cobalt retained-ß phase alloy was investigated using metallographic and X-ray diffraction methods. Hardness measurements also were made during the decomposition process. Precipitation of Ti2Co is by nucleation and growth; and an activation energy of 50,000 cal per mole was determined. The values of the coefficient ß suggest that the precipitate is pearlitic at temperatures between 450 and 475°C, and spheroidal between 500 and 525°C. THIS paper describes part of a series of invesligations into phase transformations in binary alloys of titanium with transition elements. The general approach is similar to that taken in work on titanium-iron and titanium-nickel alloys.' Previous investigators'' have established the titanium-rich end of the titanium-cobalt phase diagram, reproduced in Fig. 1. Orrell and Fontana' showed that alloys containing more than about 6 pct" cobalt quenched from the ß range, produced 100 pcl retained-p phase. The isothermal decomposition of alloys containing between 0.8 pct Co and 15.5 pct CO was investigated by the same workers in the temperature range 650 to 1000°C. They reported that these alloys transformed into a or Ti,Co depending on the cobalt content, but no quantitative data were given. In the work to be described a series of alloys containing 0.8 pct Co to 12.5 pct Co was examined in the quenched condition. The 10 pct Co alloy (the lowest cobalt content to retain 100 pct ß on quenching) was selected for further work on the tempering kinetics of the ß decomposition. Experimental Procedure Since our own melting equipment was not installed at the outset of this work, the Physical Metallurgy Division of the Department of Mines and Technical Surveys (Ottawa, Canada) prepared the alloys. These were made of Japanese sponge, (which when melted had a value of 103 DPH, using a 1-kg load), and electrolytically prepared cobalt. The al- loys, made up to contain 0.8, 1.6, 3.3, 5.8, 8.3, 10.0 and 12.5 pct Co, were homogenized by swaging into rods at 900°C. Filings were taken from the rods, and any iron chips from the file were separated magnetically. Size fractions of both plus and minus 200 mesh (about 75p) were shown by their constitution, after annealing just below the eutectoid temperature, to contain the same cobalt content. Consequently, it was permissible to use the —200-mesh fraction, knowing it to be representative of the rod composition. Quenching in argon was carried out in a newly designed furnace, whose features include (1) an Inconel furnace tube, (2) a positive pressure of argon maintained at all times in the furnace—even when a sample is removed or inserted. The furnace is shown in Fig. 2 and is described in the Appendix. The tempering processes were carried out on powder samples sealed in evacuated quartz capsules. Since the highest tempering temperature was 525OC, no protection against reaction with the quartz was necessary. (Tests were made on filings of iodide titanium and showed no hardness increase after equivalent heat-treatments.) A thermocouple was attached to the capsule, which was heated to the

Jan 1, 1959

By Rex B. McLellan, W. A. Oates, William W. Dunn

Vapor transport experiments have been carried out in order to determine the saturation solubility of carbon in cobalt and nickel with respect to graphite over a large temperature range. Some of the uncertainty existing in the thermodynamics of these systems has been removed and accurate estimates of the heat and entropy of solution of carbon in nickel and cobalt have been deduced. The relatitle partial entropies of carbon are considered to be predominantly vibrational in origin. ALTHOUGH the thermodynamic properties of solid solutions of carbon in cobalt and in nickel have been investigated previously, the results of these investigations show a marked lack of agreement amongst themselves. In this investigation simple vapor transport experiments have been undertaken in order to measure the temperature variation of the saturation solubility of carbon in nickel and cobalt with the object of removing to some degree the uncertainties in the thermodynamics of these systems. In the case of the C-Co system, early measurements of the saturation solubility of graphite in Co show results at the same temperature differing by almost an order of magnitude.1-5 Recently Schenck, Frohberg, and Jaspert6 measured the equilibrium between CH4-H2 mixtures and C-Co solid solutions at five temperatures ranging from 850° to 1050°C. Their values of the activity of carbon in the solid solution, deduced from a knowledge of the chemical potential of carbon atoms in the gas, varies linearly with composition at each temperature and the authors concluded that the solutions were Henryan. The saturation solubilities deduced from Schenck, Frohberg, and Jaspert's measurements are in good agreement with the solubility determined at 1000°C by Rao and Nicholson7 and the value at 1000°C deduced from the measurements of smith8 on the equilibrium between CO/CO2 mixtures and C-Co solutions. The object of this investigation was to check the results of Schenck, Frohberg, and Jaspert and also to extend the range of solubility data to higher temperatures. In the case of the C-Ni system, there is fairly good agreement between the values given by schaefer9 for the saturation solubility of carbon C, in nickel, the value given at 1000°C by Rao and Nicholson,7 and that deduced from Smith's8 measurements of the equilibrium between C-Ni solutions and CO/CO2 mixtures at 1000°C. The values of C, deduced from Schenck, Frohberg, and Jaspert's6 measurements of the carbon activity in nickel are also in fairly good agreement. However, there is a large discrepancy between the above set of measurements and those of Lander, Kern, and Beach," who measured the carbon solubility of nickel in equilibrium with graphite by depositing an excess of graphite on the surface of Ni-foils from a gaseous mixture and subsequently diffusing in the carbon. These results are considerably higher than those mentioned above. The determinations6 of carbon activity a, in nickel from the CH4-H2 equilibrium showed that at all the temperatures investigated, the ac-values varied linearly with concentration up to about a, = 0.6 and then began to increase with concentration much more rapidly. On the basis of auxiliary experiments in which C-Ni solutions were equilibrated with graphite, Schenck, Frohberg, and Jaspert concluded that their CH4-H2 solid equilibrations at high values of a, were spurious and a, behaved linearly with composition up to the saturation limit (a, = 1). The short linear extrapolations of Schenck, Frohberg, and Jaspert's a, data yield values of C, in good agreement with those of Lander, Kern, and Beach." The solubility data for nickel discussed here is presented in Fig. 1 in the form of plots of ln[Cc/(l - 2cc)] vs 1/T. The discrepancies mentioned are clearly seen. In this investigation a vapor transport method is used to measure C, over as wide a temperature range

Jan 1, 1969

By C. H. Li, J. Washburn, E. R. Parker

Yield stress in single crystals of zinc was shown to be dependent on prior annealing temperature and rate of cooling after annealing. Rate of strain hardening beyond the yield was not sensitive to annealing procedure. A tentative mechanism for the effect was discussed. COMPARATIVE mechanical tests of metal single crystals generally show a large scatter of results. Many factors may contribute to this variation. The present investigation was undertaken to evaluate the influence of two factors not ordinarily considered of major importance—annealing temperature and cooling rate after annealing. Since plastic properties of crystals are thought to depend on the presence of lattice imperfections, it follows that a variation in properties should result from differences in the distribution and density of these imperfections. Furthermore, in the light of current theories of interaction between edge dislocations and lattice vacancies,' it seems possible that annealing temperature and subsequent rate of cooling might play a part in this distribution. Analysis of the effect of these variables on plastic properties may lead to a better understanding of the annealed state. Single crystals of zinc which have been strained in simple shear undergo complete recovery of mechanical properties upon subsequent annealing. This behavior is useful because a single specimen can be used repeatedly, thus eliminating the uncontrollable variables introduced by the use of many crystals. The test section of the crystals used for these experiments was a cylinder 1/8 in. thick with a cross-sectional area of about 1/3 sq in. The specimens were acid-machined from spherical single crystals 1 in. in diameter in such a way that the slip plane (0001) was at right angles to the axis of the cylinder. In testing, a shear stress was applied along one of the slip directions, [2110] in the (0001) plane.' All crystals, unless otherwise noted, were grown in a helium atmosphere from molten 99.99 pct pure Horse Head Special Zinc. Fig. 1 is a family of curves obtained from one crystal. Each curve was obtained by deforming the crystal to 10 pct strain at a rate of 3 pct per min, following an anneal of 1 hr at 260°C. The strain direction was reversed every other time so that no progressive change in shape of the specimen took place during the series of tests. Since the stress-strain curve was reproducible within a fairly narrow range under the same conditions of annealing, it was then possible to determine the effect of changes in annealing conditions. A crystal was tested repeatedly as previously described but the annealing temperature and rate of cooling preceding each test were varied (Fig. 2). Two cooling rates were used, approximately 30°C per min and 3°C per min. Annealing was conducted at three temperatures, 200°, 300°, and 400°C. For a given annealing time and rate of cooling the room temperature flow stress was higher the higher the annealing temperature. The increase in flow stress was small as the annealing temperature was increased from 200° to 300°C but rose rapidly when the annealing temperature was raised from 300" to 400°C. Faster cooling from the high temperature produced an even greater strengthening of the crystal. The curves were obtained in the order indicated by the numbers. The stress level associated with a certain annealing treatment was, within the limits of scatter, always the same regardless of the

Jan 1, 1954