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By L. S. Allen, R. L. Caldwell, W. R. Mills

Borehole models used in the study of nuclear well logging are reviewed and the merit of heterogeneous us homogeneous formation simulation is discussed. .A heterogeneous model for simulating sandstone formations of variable porosity is described. Simulation adequacy was checked by steady-state and pulsed-neutron measurements. INTRODUCTION In the course of developing new methods of nuclear well logging, the problem of testing new logging instruments under controlled conditions always arises. This testing is usually done in wells of known lithology, porosity and fluid saturation, or in laboratory test facilities which simulate the borehole environment. Although the former approach is possibly more satisfying, it is frequently difficult or inconvenient to find wells with enough variation in the cited parameters for a truly comprehensive study, On the other hand. laboratow- test facilities can simulate a wide variety of formation and borehole conditions if care is exercised to maintain adequate simulation under all conditions. Workers concerned with the development of nuclear well logging methods have reported several types of research facilities in the past. Tittle, et a1 used cubical tanks filled with Ottawa silica sand to study the steady-state behavior of thermal and epithemal neutrons in simulated sandstone logging environments.1 In addition to the effects of fresh vs salt water, a wide variety of casing sizes and compositions were investigated. Tittman also used a large tank of Ottawa sand to measure the slowing down length of sio2;2 for making the same measurement in CaCO3, however, an assembly of solid Vermont marble blocks was used. More recently a very useful and carefully planned test pit for nuclear logs was constructed under the auspices of the API.3 This facility consists of three massive limestone sections, each 6-ft thick and more than 5 ft in diameter. The blocks are buried, one on top of the other, in a concrete- lined pit having a total depth of 24 ft. Each section is made of a different limestone to achieve porosity variation, the selection being Carthage (2 per cent), Indiana (19 per cent) and Austin (26 per cent). The blocks are traversed by a 7 7/8-in. diameter borehole and are saturated with fresh water. Great care was taken to insure total saturation of the stone. Homogeneous mixtures and materials have not been used exclusively for simulating earth formations. Tittle, et a1 4 showed that a heterogeneous lattice of water and graphite could be used to simulate Liquid furfural with very little effecton measured thermal and epi thermal neutron distributions. Subsequently, a lattice-type model for simulating limestone earth formations was designed and built by Berry This limestone model was constructed of 7/8- x 11/4- x 36411. marble rods glued together with a plastic resin to form a 36-x 42- x 42in. cube. The cube was honeycombed vertically with 7/8- x 7/8- x 3641-1. holes for porosity and had a 111/2-in. diameter hole in the center to serve as the borehole. Lower porosities were simulated by placing marble rods in the square holes. The finished cube was used with the borehole vertical and set in a tank to hold liquid for filling the holes in the rock matrix. A second type of heterogeneous borehole model has been proposed by Kukharenko, et a1.6= In this concept the model is composed entirely of solid material. The hydrogen equivalent of formation fluids is simulated by making the model of alternating layers of dense rock and celluloid. Additional hydrogen is included by drilling vertical holes in the rock sections and filling them with solid forms of hydrogeneous material. The volume of the holes is equal to the volume of the celluloid layers, so an axial and radial dispersion of the hydrogeneous material is thus obtained. One such model was composed of alternate 50 mm-thick sand layers and 2 mm-thick celluloid sheets. Approximately 200 appropriately spaced plastic tubes were used in each sand section. The plastic tubes were filled with paraffin for additional hydrogen concentration. This arrangement yielded a model with a water-equivalent hydrogen concentration of 10 per cent. Experimental data taken in this model and in a model consisting of the same material but homogeneously dispersed showed that the heterogeneous system adequately

Jan 1, 1966

By H. G. Moulton

The increasing scale of mining operations over the past decade, particularly in connection with the exploitation of large bodies of comparatively low-grade copper ores, has made necessary the study of the behavior of rock under failure. When extractions of as high as 40,000 tons a day are reached in steam-shovel operations and as high as 20,000 tons per day in underground mining operations, it is evident that excavations soon become of such size that the behavior of the rock will often be dependent on fundamental principles applicable to more or less homogeneous materials under stress, rather than on weathering or local planes of weakness. In the ordinary rock excavations encountered in civil-engineering practice, such as excavations for subways, highways, railroads, etc., rock faces are not carried to depths sufficient to develop any pressures, or consequently any failures, except those due to loose masses resulting from local planes of weakness. When, however, orebodies whose tonnage is measured by hundreds of thousands are to be extracted by steam-shovel operations in open pits, it is necessary to determine if possible in advance the slopes that the sides of the pits will assume, for these slopes influence the shape of the excavations and thereby the amount of ore that may be extracted by the open-pit method. When large orebodies are mined underground at depths of 300 to 500 ft. (91 to 152 m.) by caving methods, the surface subsiding as the ore is withdrawn, it is necessary to determine in advance the outermost limits of fracture in the subsiding surface, for on the delineation of these limits depends the location of surface improvements, mills, smelters, etc. and also the location of development work, such as hoisting shafts, main haulage levels, and all other underground openings that must remain undisturbed during the period of ore extraction. Heretofore, in civil-engineering practice, it has been assumed that earth and rock behave differently in failure. For the calculation of earth pressures, formulas are used in which the assumption is made that earth banks fail by sliding along the slope determined by the frictional resistance of the material. The line of failure and the resulting pressure is held to be dependent on the angle of repose, which is different for varying

Jan 1, 1920

By A. H. Daane, B. J. Beaudry

The Sc-Y and Sc-Zr systems were studied by thermal and X-ray methods. Both systems are characterized by complete solid solubility in the low temperature hexagonal form and in the high temperature bcc form. In the Sc-Y system, there is a minimum in the solidus at 50 at. pct and 1365°C, while the solidus in the Sc-Zr system follows a nearly straight line relationship between the melting point of scandium and zirconium. There is a minimum in the temperature of transition from hexagonal to bcc in the Sc-Y system at 43 at. pct Y and 1175°C; while the temperature of transition is raised in the Sc-Zr system to a maximum of 1415 °C at 30 at. pct Zr. INTEREST in the metals of the first transition series has usually stemmed from their useful properties; however, there is now a great deal of interest in determining the fundamental nature of these metals. Since scandium is the first of these transition metals, a study of the preparation and Properties1 and the alloying behavior of scandium2 was initiated. In a continuing study of the alloying behavior of scandium, the systems of scandium with zirconium and yttrium have been established. Extensive solid solubility in both the Sc-Zr and Sc-Y systems was expected from application of the classical rules of Hume-Rothery. Also, the modified Darken and Gurry plot as suggested by Gschneid-ner3 showed ideal conditions for solubility in the Sc-Zr system with less favorable conditions in the Sc-Y system. The effect of scandium on the transformation temperature of zirconium and yttrium was of interest, since a recent empirical observation by Uly and Burr4 predicted that the solute scandium would raise the transformation temperature of zirconium and lower the yttrium transformation. In addition to noting the validity of the above predictions, the SC-Y and Sc-Zr systems were established. EXPERIMENTAL METHODS Materials. The metals employed in this investigation were crystal bar zirconium, distilled scandium prepared by the method described by Spedding, et al.1 and yttrium prepared by the method described by Carlson, et a1.5 The major impurities present in these metals are listed in Table I in ppm. Alloy Preparation. All the alloys examined were initially formed by comelting the two metals in a nonconsumable electrode arc-melting furnace under an atmosphere of purified helium or argon. The buttons were inverted at least five times and re-melted each time to ensure homogeneity. During preparation of Sc-Zr alloys, approximately 1 wt pct was lost which was attributed entirely to the loss of scandium by distillation. When preparing Sc-Y alloys, approximately 1.5 wt pct was lost, but it was assumed that the intended composition was maintained, since the relative weight lost when arc melting the component metals was nearly the same. Samples weighing 15 to 20 g were prepared for time-temperature thermal analysis, while only 1- to 2-g samples were prepared for the optical pyrometer and X-ray diffraction studies. Thermal Methods. The solidus and the melting points of the metals were determined by an optical pyrometer method described previously.2 The temperatures at which the transformation from hexagonal to bcc occurs were determined by differential thermal analysis. Several points on the solidus and liquidus in the Sc-Y system were also determined by this method and are in good agreement with those obtained by the optical pyrometer method. The procedure followed in the preparation of samples for thermal analysis and the furnace used have been described elsewhere.2'6 Since a limited quantity of scandium was available, most of the alloys were not melted during thermal analysis, thus avoiding contamination by the crucible. The alloy could then be reused and the composition changed by adding the desired quantity of solute to obtain the next alloy. Heat Treatment and X-Ray Methods. In order to ensure homogeneity, the "as arc-melted" alloys Were wrapped in tantalum foil, sealed in quartz capsules and heated at 1100°C for 15 hr and then cooled at a rate of 8 deg per min. Samples for X-ray diffraction were filed from these heat-treated alloys, sealed in 1/8 in. by 1/2 in. tantalum capsules under

Jan 1, 1963

By J. E. Lamar, J. S. Machin

INSULATING materials include a wide variety of nonmetallic mineral products such as exfoliated vermiculite, expanded gypsum, 85 pct magnesia, diatomite, asbestos, perlite, cellular glass, pumice, silica aerogel, expanded aggregates and mineral wool. Except mineral wool, most of these products, or the materials from which they are manufactured, are described in other chapters of this book. PROPERTIES OF INSULATING MATERIALS The insulating properties of the materials considered in this chapter result in general from entrapping extremely small pockets of air in such a manner that heat is not transferred by convection. The minimum heat conductivities of such insulating materials are slightly greater therefore than the conductivity of still air. In addition, conductivity varies with the overall density of the material, the temperature range in which the measurements are made, and the form into which the material is fabricated. However, the numerical value of heat conductivity should not be the sole criterion of an insulating material; for a particular application it may be advantageous to use a material of somewhat higher conductivity in order to secure other desirable engineering properties. This is especially true with certain materials that are used because of their refractoriness. Comparative insulating values of some commonly used insulating materials are shown in Table 1. In comparing the values presented in this table it should be borne in mind that heat conductivity varies with the mean temperature, with the overall density, and with the amount of moisture present. With fibrous or granular materials it varies with fiber or grain size and with the amount and kind of binder, if any is used. Under some circumstances it may vary with the arrangement of

Jan 1, 1949

By John Gann

THE following investigation constitutes a brief resume of the more important binary magnesium alloys from the standpoint of metallographic technique, and the effect of heat treatment on structure and properties. The comparative newness of the subject justifies this procedure as a preface to a more detailed study of each individual series of alloys. The work was started with the idea of practical application in the industry rather than as a theoretical investigation. The alloy compositions studied were selected as those most likely to show whether heat treatment would produce beneficial results. Furthermore, it was considered satisfactory to use commercial 99.9 per cent. magnesium, the best commercial grade of alloying ingredients, and to limit the time of heat treatment at the expense of incomplete equilibrium. These facts must be kept in mind when examining the results obtained, and the conclusions drawn.

Jan 1, 1928

By O. D. Gonzalez, H. A. Wriedt

Alloys ranging from pure iron to pure nickel were saturated with nitrogen gas at 918°, 999°, and 1217°C and analyzed. The solubility of nitrogen at 1-atm pressure was obtained as a function of nickel content for the whole range of iron-nickel alloys and the temperature dependence of solubility is shown for the experimental alloy compositions. The heat of solution and the entropy of solution of nitrogen in the alloys as func-tiom of composition up to 41 pct Ni are given. 1 HE acquisition of more exact thermodynamic information for systems composed of iron with various alloying elements continues to interest ferrous metallurgists. The interstitial alloying elements, especially carbon, hydrogen, and nitrogen, comprise a field of particularly intense study. A recent investigation of carbon solubility in Fe-Ni alloys held at 1000°C in gases of fixed carbon activity showed an unpredicted minimum in the solubility near 72 pct Ni.1 The present investigation was undertaken to see if a similar anomaly in solubility existed for nitrogen in Fe-Ni alloys. The solubility of nitrogen in ? iron at known nitrogen activities has been measured several times.&apos;-&apos; Corresponding information for the solubility of nitrogen in solid Ni and Fe-Ni alloys is not available. Juza and sachsze9 reported that metallic nickel dissolved 0.07 pct N in equilibrium with Ni3N at 445°C. This result was regarded as dubious by Turkdogan and Ignatowicz10 who found less than 0.0004 pct N in nickel specimens equilibrated at 600°C with ammonia-hydrogen mixtures having fugacities of N2 gas up to 35,000 atm. Such fragmentary reports indicate only that nitrogen gas has a very much lower solubility in nickel than in iron. MATERIALS A purified iron from Battelle Memorial Institute was used for solubility measurements. This grade contained more than 99.95 pct Fe, the highest content of any measured individual impurity being 50 ppm for each of As, C, Cu, and Pb. The nickel and iron-nickel alloys, supplied by the International Nickel Co., contained 0.02 to 0.04 pct C, 0.17 to 0.19 pct Mn, 0.04 to 0.08 pct Si, < 0.01 pct P, <0.03 pct S, and <0.20 pct Co as principal impurities. The Fe-0.59 pct Mn alloy was of zone-melted quality, the highest concentration of any individual impurity being 15 ppm Al. The "prepurified" grade of nitrogen gas from Matheson Co. had a nominal nitrogen content of 99.996 pct. An "electrolytic" grade of hydrogen gas from National Cylinder Gas. CO. in which the principal impurity is water vapor was admixed with the nitrogen to prevent oxidation of these specimens. This grade was preferred to a purer grade because the presence of some oxygen helps in suppressing contamination of the specimens, for instance, by silicon from the porcelain furnace tube. EXPERIMENTAL PROCEDURE The specimens were equilibrated in vertical tube furnaces through which a 99 pct N2-1 pct H2 gas was passed at ambient pressure. For the 915", 918", and 999°C runs, a wound-resistance furnace was used, and for the 1217°C runs, a furnace with a tubular silicon carbide element was used. The temperature control system on both furnaces was similar: a Weston "Celectray" controller with a modulator, responding to the electromotive force of a thermocouple with its hot junction in the furnace, switched the furnace current between high and low settings. The temperature distributions in the working zones of the furnaces were determined with calibrated Pt/Pt-10 pct Rh thermocouples. The overall uncertainty in temperature was estimated to be ±3° at 915° to 999°C and ±5° at 1217°C . Consideration of the small temperature coefficients of the equilibria studied, together with the error limits in the method of analyzing for nitrogen, showed that further refinement in temperature uniformity would give no improvement in resultant accuracy. The reactive gas was generated by mixing together "prepurified" nitrogen and "electrolytic" hydrogen directly from cylinders commercially supplied. The flow rates of nitrogen and of hydrogen were fixed by setting with bleeders the pressure drops across the individual calibrated flow meters of constant resistance. For any given alloy, the solubility of nitrogen at 1-atm pressure (% N) was obtained from the analyzed nitrogen content of equilibrated specimens (% Na)according to Sieverts&apos; law, thus

Jan 1, 1962

By Philip D. Wilson

IT has been my privilege to read the article prepared by R. S. Dean entitled "Production of Alumina from Low-Grade Domestic Materials" which appears on another page of this issue. Dr. Dean should be congratulated on the preparation of such an erudite and scholarly dissertation on bauxite and on the work which the Bureau of Mines has been doing in connection with the development of processes to use low-grade domestic materials.

Jan 1, 1943

By W. D. Ludemann, J. E. Dor, L. A. Shepard

Recovery of the creep resistance of 99.99 pct pure Al was studied at temperatures 540°, 573°, 600°, and 611°K. Poly-crystalline specimens crept under a stress of 950 psi to a strain of 5.5 pct were allowed to recover for periods of from 1 min to 16 days under a residual stress of 4.4 psi. Increased creep rates upon reapplication of the 950 psi stress evidenced softening of the material. The activation energy for the recovery process was found to be 64,000 cal-per mol. THREE major observations have clearly revealed that the creep of polycrystalline aluminum above about 510°K is controlled by the rate of climb of jogged edge components of dislocations past the barriers impeding their motion: 1) Extensive polygonization, characteristic of climb, takes place during creep.&apos;9&apos; 2) The activation energy for creep equals the estimated activation for self-diffusion. 3) The stress law for creep coincides with theoretical predictions based on the climb mechanism.4,5 The decreasing rate during the primary stage of creep must be ascribed to the introduction of additional barriers to the glide of dislocations. During secondary creep the density of barriers must remain constant, the rate at which new barriers are formed being equal to the rate at which they recover. For this reason the nature of the barriers, and their rates of formation and recovery, are significant to a complete understanding of creep. It is proposed here to study the kinetics of the recovery of barriers to creep of high-purity polycrystalline aluminum in the climb range. The technique will consist of creeping a series of tensile specimens under a prescribed stress to given state following which the specimens will be recovered for various times and temperatures under approximately zero stress. The amount of recovery will be determined by comparing creep curves following the recovery. EXPERIMENTAL PROCEDURE The material used for this investigation was a 99.99 pct pure Al supplied by the Aluminum Co. of America in sheets of 0.001-in. thickness having an H-18 temper. The spectroscopic analysis of impurities gave Cu-0.004 wt pct, Fe-0.002 pct, Si-0.001 pct, others-0.000 pct. Creep specimens were machined with their tensile axes in the rolling direction of the sheets. Annealing in a molten potassium nitrate-potassium nitrite bath for 1 hr at 686K, followed by air-cooling, resulted in a grain diameter of from 0.22 to 0.27 mm. Creep machines were equipped with constant stress lever arms of the type suggested by Fullman, Carreker, and Fishher,&apos; which maintained the applied stress to within 0.04 pct of the reported value of 950 psi. Creep strains were calculated from extensions over a 6-in. gage section to the nearest 3 X 10"5. The temperatures of testing, 540°, 573", 600°, and 611°K, were obtained by immersing the specimen and extensometer assembly in a molten KNO2-KNO3 bath. Temperatures during the periods of creeping could be maintained constant to within better than ± 1°K. Correlation of creep data at different temperatures of testing demanded the use of an appropriate temperature-compensated time 8. Previous investigations have shown that the creep of pure metals at temperatures above about 0.55 of their melting temperatures can be correlated by the functional relationship3" e=f(0), s= const. [1] where e = total plastic strain during creep f = a function that depends on stress a = stress 6 = te-Q/RT = a temperature-compensated time t = time under test Q = 35,500 cal per mol = activation energy for creep R = gas constant, and T = absolute temperature In the present series of tests all of the creep was conducted under the same stress of 950 psi. To provide identical initial conditions for the recovery all specimens were first crept to a temperature-compensated time of = 47 X 10-14 min which resulted in a creep strain of 0.055 + 0.005 regardless of the creep temperature. During recovery, a small stress (4.4 psi) was permitted to remain upon the specimens to maintain tautness in the pulling assembly and to prevent mechanical damage to the soft specimen. After each recovery period, the full stress was reapplied and

Jan 1, 1961

By Smith Bracewell

First evidence of bauxite in Jamaica resulted from an analysis of a soil sample collected at Bull Savannah in 1938 during a systematic local investigation of the island&apos;s soil types. Results of subsequent work indicated the possibility of the occurrence of deposits of commercial grade and dimensions, and in 1942, with a view to emergency development of the deposits as a war measure, the Jamaican Government declared all bauxite in the colony to be Crown property.

Jan 10, 1958

By R. K. Hopkins

For a great many years fusion welding has been used in and around petroleum refineries, but it is only within six or seven years that the more important pressure vessels have been constructed by this process, because before that time the properties of fusion welds would not with-stand such rigorous service. Since the adoption of fusion welding for the construction of this equipment, the refiner has required pressure vessels suitable for operation over a very wide range of conditions. On the one hand, vessels must operate at extremely high temperatures, in the range of 950° to 1000° F., and on the other vessels must be suitable for operation at sub-zero temperatures down as low as -75° F. Also, vessels are required suitable for operation at pressures upwards of 1000 lb. per sq. in., and as low as a 29-in. vacuum. In addition, vessels are required to withstand the attack of very corrosive mediums. It has been a rather difficult task for the fabricator to meet all of these require-ments, but as a result of the extensive research carried on by steel manu-facturers and several fabricators of class I vessels, practically all of these demands have been met. In order to meet the refiners&apos; requirements for this wide range of conditions, the fabricator has worked closely with the metallurgist. This has enabled him to choose the proper base metal for each service condition, but it has been the fabricator&apos;s problem to develop a welding rod and welding technique, as well as a heat-treatment, that would produce in the welded vessel characteristics in and around the weld comparable to those in the base metal. Where corrosion is not a serious problem, and where the operating temperatures are not too high, ordinary carbon steel has served very well. But when corrosion is serious, and/or when the temperatures are either very high or very low, it is necessary to use some form of alloy steel to give satisfactory service.

Jan 1, 1935

By H. S. Martin

ALTHOUGH it was known some years ago at the- Utah Copper Co. mills that fine grinding improved flotation recoveries, no accurate data were available until recently as to just how far the grinding could be carried economically. In 1923 the ultimate degree of fineness for flotation feed was supposed to be about 10 per cent. on 65 mesh, with approximately 55 per cent. through 200 mesh, which meant that most of the mineral would pass 100 mesh. At this time Garfield and Wilfley tables were used ahead of flotation and a good deal of the coarse mineral removed prior to the ball mill regrind. Shortly afterwards, mill-scale tests developed the fact that on a feed containing not over 10 per cent. +65¬mesh material flotation alone would give a copper recovery equal to that obtained by the combination of tables and flotation, but that on much coarser feed the recovery with flotation alone was lowered. This was at a time when all the sulfide minerals were floated if possible, so that the only requisite was to grind fine enough to free the mineral from gangue. EARLIEST USE op MICROSCOPIC EXAMINATION OF TAILINGS As early as 1921, the writer had attempted to determine by chemical analysis the relative proportions of copper minerals in tailings from an ore that made extremely poor flotation results. Chemical analysis was not satisfactory or conclusive, and samples of these tailings were sent to the U. S. Bureau of Mines Station at the University of Utah for micro-scopic examination. The question at that time was to determine, if possible, which copper minerals had been lost and why, but R. E. Head, in his report, revealed other interesting data. He said in part: Briefly stated, the mineral particles or grains may be classified into separate groups as follows: 1. Free grains of pyrite, chalcopyrite, chalcocite and bornite, respectively, which contain no other included sulfides; 2. Grains in which all three of the copper sulfides are represented (the core may he of chalcopyrite, partially altered to bornite, these two minerals being entirely surrounded by a shell of chalcocite); 3. Grains composed of equal amounts of bornite and chalcocite or chalcopyrite and chalcocite.

Jan 1, 1929

By E. Gaujot

IN connection with the question of coal waste and economy in mining, we would call the attention of those interested to an apparatus invented by M. Dernencourt, Superintendent of the Anzin Division of the Anzin Coal Company, North of France. This apparatus is known in France and Belgium under the name of prop screw jack (vis botte), and has been used with good results in the above-named countries for some years past. M. Ponson gives, in his " Traité de l&apos;exploitation des Mines," a description of it (page 533), but as the description given is old, the work not widely known in this country, and as some valuable improvements have been made since, I thought it might be useful to give a description of it, having seen it in operation in 1867, while in Europe to attend the great Exposition, and on a scientific tour to the mining districts of France, Germany, Belgium, and Italy. The prop screw jack is composed of the following pieces: I. The body or column B, Fig. 4 [Plate (1)], of oak or yellow pine, sawed square, the bark taken off, and any length, proportionate to the vein. The smallest are 10 inches diameter at the base, and 9 inches at the top, the height being from 12 to 15 inches less than the size of the vein. In the axis of this column, and at the top end, is a cylindrical opening or hole, C, 2 3/4 inches diameter, 10 inches deep, for the screw, S. II. Two wrought-iron rings, R R, to strengthen the two extremities of the column ; the rings must be put on hot. III. A cast-iron washer, E, with hole in centre a little larger than the screw, to be put on the top of the column, and on which the nut is to rest; the top side of this washer must be faced on the lathe, also the bottom of the nut, to prevent friction. IV. The screw, S, having a total length of 12 inches and a diameter of 21/2 inches (for very high veins this diameter may be in¬creased to 3 inches), and has on its top a wrought-iron plate, T,

Jan 1, 1873

By J. Gordon Parr, D. H. Polonis

High purity alloys of titanium and iron, made by a technique of levitation melting, have been investigated with particular reference to martensite formation and decomposition in the hypoeutectoid range. A preliminary study has been made of the occurrence of the phase corresponding to the structure Ti2Fe. MANY of the previous investigations of Fe-Ti alloys have been made using Kroll sponge as a source of titanium; and the subsequent heat treatments to which alloys have been subjected has, on occasion, led to further contamination. Worrier,&apos;,&apos; who suggested a part of the equilibrium diagram for the binary system, and Wallbaum and coworkers,3-5 who worked largely with iron-rich alloys, all used Kroll sponge. Van Thyne, Kessler, and Hansen,6 in their determination of the equilibrium diagram, used iodide titanium for alloys up to 30 pct Fe. Duwez,7 who measured the M. temperature of titanium binary alloys with many solute elements, used iodide titanium in all cases except in his work on Ti-Fe alloys for which he used Kroll sponge. The investigation of the supposed phase Ti2Fe by Rostoker8 nvolved the use of iodide titanium. A section of the constitutional diagram, after Van Thyne et al., is reproduced in Fig. 1. Frequently too much stress is placed on the effect of contaminants in equilibrium and nonequilibrium systems, but there is no doubt that titanium alloys are extremely susceptible to interstitial atoms. Consequently, the main purpose of the work to be described was to determine those features of phase transformations in pure Ti-Fe alloys that were considered of importance in commercial heat treatments. For, although commercial alloys may not be of high purity, the investigation of a system uncomplicated by traces of impurity is a desirable starting point. Another incidental feature, the occurrence of Ti2Fe, was also investigated. The entire study was carried out using powders obtained from alloy ingots, for diffusion reactions are often more rapid in small particles than in bulk specimens. The frequently adopted practice of ascertaining phase constitutions by X-ray analysis of powders, and relating these to the microstructures and mechanical properties of bulk specimens, is considered by the authors to be open to criticism. In the martensite reactions in the Fe-Mn system, for example, it has been shown- hat similar phase distributions in solid and powder may result in different hardness values and appearance under the microscope; and it is possible that similar anomalies might occur in the Ti-Fe system. Consequently, in order to

Jan 1, 1955

By Edward M. Weiss

THE emphasis in some political quarters on hemispheric unity and defense indicates Latin American mineral resources should be more extensively developed. However, United States mining companies have, in many instances, been discouraged by the laws of southern neighbors. At the same time, some of the countries have liberalized their mining laws in an effort to attract investments from the United States. The resultant confusion has been detrimental to all concerned. Ownership of Mineral Deposits Examination of the mining codes of Latin American countries shows that, without exception, governments reserve the right of direct ownership of all mineral resources. Ownership can be divided between the Feredal Government and the states or among the Federal Government, the states, and private individuals. However, in the majority of the nations constitutional authority vests all mineral rights solely in the Federal Government. Mexico is the only country that has expressed Federal ownership as imprescriptible; the other republics have not defined the exact significance of government ownership. The implication derived from the general economic and political climate is that all mineral resources are ultimately to be regarded as a national heritage. Whether a concession granted to an individual or corporation carries any right of private property is shaded with a variety of meanings. The exceptions at one extreme are Argentina and Bolivia, whose laws state explicitly that a concession granted to a juridical person is an act of the state, and the land becomes the private property of the individual, and the concessions constitute real property. However, in Mexico mining concessions or grants do not create rights of fee-simple ownership. The concession only conveys the exclusive right to explore, develop, and work the deposits. The mining property remains the property of the state. In some instances exploitation concessions represent a compromise between private and government ownership. In Honduras the period granted to a mining enterprise is fixed at 90 years. At the end of that time, the enterprise and all installations revert to the state without compensation.

Jan 1, 1952

By P. M. Kelly, E. P. Butler

Four Mn-CLL alloys, containing 60, 70, 80, and 90 pct Mn, respectively, have been examined in the quenched and the quenched and aged conditions using electron microscopy and electron, neutron, and X-ray diffraction. After certain heat treatments the alloys transform from fee to fct and in the tetraom1 condition show a domain structure parallel to {101} planes. Neutron diffraction indicates that the domains are antiferrornagnetically ordered. The domain boundary contrast has been examined using bright- and dark-field microscopy, and the contrast effects observed under favorable conditions have been used to deduce the c axis orientation in each domain. The domains are extremely mobile and can be nucleated at precipitate particles and screw dislocations. The domain mobility is responsible for the high damping capacity. In the aged material a Mn precipitates in the Kurdjumov-Sachs orientation and results of both electron microscopy and neutron diffraction indicate that the matrix separates into two components—one rich in manganese and the other rich in copper. ALLOYS of manganese and copper have the unusual combination of a high damping capacity and good mechanical properties and have been the subject of a number of investigations as part of a general interest in high damping capacity alloys for engineering purposes.&apos;,&apos; SO far, however, there has been no reported electron metallographic study of these alloys. The Mn-Cu system has an extensive range of solid solubility at high temperatures, and the equilibrium phases are expected to be y (fee) and a Mn. The high damping capacity is associated with a metastable tetragonal structure of variable c/a ratio, which forms from the high-temperature y phase. This latter phase becomes more difficult to retain as the manganese content increases, and alloys containing more than 82 wt pct Mn undergo a reversible martensitic fcc — fct transformation on quenching. The X-ray work of Basinski and christian3 showed that the Ms temperature for the transformation was below room temperature for alloys in the range 70 to 82 pct Mn and increased linearly with manganese content. When quenched from the y region, alloys in the range 50 to 82 pct Mn are cubic at room temperature, but become tetragonal if aged at temperatures between 400" and 600°C. The martensite transformation occurs on cooling from the aging temperature. Tetragonal alloys have a banded microstructure and the bands analyze to be traces of (110) planes. Similar microstructures have been observed in In-Tl4 and in other manganese-base systems, such as Mn-Au5 and Mn-Ni.6 The mobility of the bands in Mn-Cu alloys can be demonstrated by optical examination of a polished specimen surface subjected to a cyclic stress.7 The bands appear and disappear as the stress is varied, and X-ray measurements of the (200,020) and (002) peak intensities confirm that a reversible reorientation of the tetragonal structure occurs. Meneghetti and sidhu8 investigated the magnetic structure of Mn-Cu alloys and found antiferromagnetic ordering in furnace-cooled alloys of composition >69 at. pct Mn. Magnetic super lattice reflections occurred at the (110) and (201) positions and the proposed structure was fct with the spins along the c axis. A more complete investigation by Bacon et al.9 confirmed this structure. The magnetic ordering temperature Tn was found to increase linearly with manganese content in the same way as the Ms temperature, and at any composition, Tn > Ms. This relationship suggested that the magnetic ordering was responsible for the cubic — tetragonal transformation in the manganese-rich alloys. The purpose of this investigation was to study the mechanism of high damping and the structural changes that occur on aging. The main technique used was transmission electron microscopy, but X-ray and neutron diffraction experiments were also carried out. EXPERIMENTAL Materials and Heat Treatment. The four alloys, provided by the Admiralty Materials Laboratory. were of nominai composition 60, 70, 80, and 90 Mn and all had low impurity levels, <0.05 pct C, <0.2 pct Fe. This material was cold-rolled to 200-µ strip with intermediate annealing and then given a final heat treatment of 24 hr in the range 800° to 900°C followed by water quenching. An identical heat treatment was given a length of 3/4-in.-diam bar of the 70/30 alloy from which the neutron diffraction specimens were machined. It was suspected that the tetragonal structures would be metastable at room temperature, and so the alloys were not aged until required for experiments. After aging in a salt bath the alloys were water-quenched. Thin Foil Preparation. Initial thinning to 50 to 75 µ was possible in a solution consisting of: 50 ml nitric acid 25 ml acetic acid 25 ml water The surface deposit and grain boundary etching was removed by a final electropolish at around 20 V in an electrolyte consisting of:

Jan 1, 1969

By R. B. Gilmore

The North Texas district, as herein defined, includes the counties of Archer, Baylor, Clay, Cooke, Foard, Hardeman, Jack, Kiiox, Montague, Wichita, Wil-barger, and Young. Jack and Young Counties are included for the first time so that this district will correspond with District No. 9 of the Texas Railroad Commission. This area covers generally the crest and south flank of a system of buried mountains known as the Red River uplift. The oil and gas accumulations along this feature are in traps, which, although localized by structures incident to the regional uplift, usually are modified by stratigraphic changes in the sediments. The structural deformation caused by the Red River uplift is modified by the Rend arch, which is a broad anticline plunging northward from the Llano uplift in central Texas through Young and into Archer Counties. The fields in southern Archer, southeastern Baylor, southwestern Clay, and western Jack Counties arc on the extreme north end and along the flanks of the Bend arch and have generally the same type of oil and gas accumulation as the other fields in this district. Recent exploration has been along the flanks of the Fort Worth syncline, which is east of the Bend arch and south of the Red River uplift and extends into southeastern Clay and southwestern Montague Counties and along the eastern part of Jack County. The larger part of past oil and gas produc- tion has come from Pennsylvanian strata, with less important amounts lrom the Permian, and minor quantities from the Mississippian and Ordovician. Developments during 1943 About 1100 wells were drilled in the district during 1943 and more than 500 oil wells were completed, an increase from 1942. of approximately 12 per cent in the number of successful drilling operations of the total wells drilled. The addition of Jack and Young Counties to this district accounts for part of this increase, almost 150 wells being completed in the two counties. Production increased slightly over the previous year as a result of an increase in the number of producing wells and a greater demand for this high-gravity, sweet crude oil. The average depth of discovery wells was about 400 ft. deeper than in 1942. Although more discoveries produced from horizons below the base of the Strawn series than from those above the Straw, the deeper horizons, including the Bend series of the Pennsylvanian, the Mississippian limestone and Ellenburger of the Ordo-vician, largely were dissappointing from the viewpoint of major additions to oil reserves. The largest single addition to the reserves was in the basal Strawn sand in the Walnut Bend field, Cooke County. During the year, 31 wells were completed, both in the field and as cxtensions. The most active arca Was Jack County, in which five fields or potential fields were discovered, although only 44 oil wells were completed.

Jan 1, 1944

By R. B. Gilmore

The North Texas district, as herein defined, includes the counties of Archer, Baylor, Clay, Cooke, Foard, Hardeman, Jack, Kiiox, Montague, Wichita, Wil-barger, and Young. Jack and Young Counties are included for the first time so that this district will correspond with District No. 9 of the Texas Railroad Commission. This area covers generally the crest and south flank of a system of buried mountains known as the Red River uplift. The oil and gas accumulations along this feature are in traps, which, although localized by structures incident to the regional uplift, usually are modified by stratigraphic changes in the sediments. The structural deformation caused by the Red River uplift is modified by the Rend arch, which is a broad anticline plunging northward from the Llano uplift in central Texas through Young and into Archer Counties. The fields in southern Archer, southeastern Baylor, southwestern Clay, and western Jack Counties arc on the extreme north end and along the flanks of the Bend arch and have generally the same type of oil and gas accumulation as the other fields in this district. Recent exploration has been along the flanks of the Fort Worth syncline, which is east of the Bend arch and south of the Red River uplift and extends into southeastern Clay and southwestern Montague Counties and along the eastern part of Jack County. The larger part of past oil and gas produc- tion has come from Pennsylvanian strata, with less important amounts lrom the Permian, and minor quantities from the Mississippian and Ordovician. Developments during 1943 About 1100 wells were drilled in the district during 1943 and more than 500 oil wells were completed, an increase from 1942. of approximately 12 per cent in the number of successful drilling operations of the total wells drilled. The addition of Jack and Young Counties to this district accounts for part of this increase, almost 150 wells being completed in the two counties. Production increased slightly over the previous year as a result of an increase in the number of producing wells and a greater demand for this high-gravity, sweet crude oil. The average depth of discovery wells was about 400 ft. deeper than in 1942. Although more discoveries produced from horizons below the base of the Strawn series than from those above the Straw, the deeper horizons, including the Bend series of the Pennsylvanian, the Mississippian limestone and Ellenburger of the Ordo-vician, largely were dissappointing from the viewpoint of major additions to oil reserves. The largest single addition to the reserves was in the basal Strawn sand in the Walnut Bend field, Cooke County. During the year, 31 wells were completed, both in the field and as cxtensions. The most active arca Was Jack County, in which five fields or potential fields were discovered, although only 44 oil wells were completed.

Jan 1, 1944

By A. A. Smith, J. S. Smart, A. J. Phillips

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By A. J. Phillips, A. A. Smith, J. S. Smart

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By C. F. Floe, M. Cohen, M. B. Bever, V. G. Paranjpe

NITROGEN is becoming recognized as one of the important elements in ferrous physical metallurgy. Several investigations indicate that nitrogen plays a significant part in such phenomena as strain aging and temper brittleness. Nitrogen is known to be a powerful austenite stabilizer and may be a useful alloying element in stainless steels. The hard-enability of steels has been found to be increased by nitrogen. The nitriding and carbonitriding pro- cesses are examples of successful industrial application of nitrogen in ferrous materials. For a complete understanding of the various roles played by nitrogen in ferrous metallurgy a knowledge of the phase relations in the binary iron-nitrogen system is essential. The literature contains a variety of iron-nitrogen phase diagrams. Those suggested by Fry, Sawyer,² Epstein and his coworkers,³,4 Lehrer,5 Eisenhut and Kaupp, and Hägg7,8 differ significantly from one another. Moreover, the most recent of these investigations dates back about twenty years. A re-determination of the entire diagram, therefore, appeared desirable. In addition to the published phase diagrams, investigations have been carried out on portions of the iron-nitrogen system. Bramley and Haywood determined the composition and temperature of the iron-iron nitride eutectoid. The maximum solubility of nitrogen in a iron was investigated by Portevin and Seferian10 and by Diikstra. 11 Several investigators have determined the crystal structure of the various iron-nitrogen phases. In fact, Eisenhut and Kaupp6 and Hägg7 based their entire phase diagrams on the results of such studies. Epstein&apos; and Emmett12 reported lattice-parameter measurements on the E (hexagonal close-packed) phase. Osawa and Iwaisumi13 also studied the change in lattice parameters of the a, ? and E phases with nitrogen content. Brill" and Hägg7 showed that the y&apos; phase has an ordered structure, and Hendricks and Kostingsl5 suggested a structural relation between the E and phases. In a recent investigation Jackl6 arefully studied the super-lattice reflections from the y&apos; and phases. Experimental Procedure A large variety of experimental methods has been used by previous investigators in studying the iron-nitrogen system. These methods include thermal analysis, microscopic examination, X ray diffraction, magnetic measurements, dilatometric analysis and anelastic experiments. Thermal analysis is of low accuracy in determining changes in the solid state. This accuracy is further decreased for iron-nitrogen alloys since composition changes will occur during heating or cooling unless extreme care is taken to use a proper atmosphere. Metallographic methods are of small value . because homogeneous iron-nitrogen alloys of sufficient size can be produced only with great difficulty. The dilatometric method is open to the same objections as thermal analysis in that changes in composition may occur during heating and cooling. Lattice parameter measurements by X ray diffraction can be used satisfactorily for determining phase boundaries if cooling is fast enough to prevent structural changes. In view of the limitations of the various other techniques two methods only were adopted in this investigation, (1) X ray diffraction measurements, and (2) a controlled nitrogenizing method. The second method is an innovation for investigating the iron-nitrogen system, and will be described at length. Materials: All iron-nitrogen alloys were prepared from carbonyl iron powder of the analysis shown in table I. The average particle size was about 20

Jan 1, 1951