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By E. B. Harden, J. H. Harden

The practical use to which topographical models or relief-maps have been put, has within the last few years taken a wider range. They are rapidly coming into favor for other than purely scientific purposes, and their value for illustration and instruction is being more fully appreciated. Topographical maps; representing by contour-curve lines the elevations and depressions of the earth's surface, are now demanded in engineering work of nearly every description, and afford a ready means of bringing out the configuration of the country in a simple manner. A beautiful example of recent topographical mapping is seen in the seventeen sheets just issued by the Geological Survey of New Jersey. By reason of the inability of unskilled persons to understand the nature of a topographical map, it is sometimes necessary to con struct the same in relief, with the rivers, canals, railroads, etc., delin eated upon it. With the aid of such a map, problems in engineer ing science which would otherwise require expert assistance to explain them, are reduced to a simple and understandable form. Relief-maps are also of value to the geologist in working out the geological structure. To the instructor they present the most ready and efficient means of imparting clear and accurate knowledge of topography and kindred subjects. To the lawyer they are invalua ble in enabling him to bring into the court-room a representation of a part of the country with all its features accurately shown, to ex plain to the court and jury the special points about which litigation is pending and which would otherwise require long and laborious description. The application of the topographical map to business purposes is shown in a relief constructed by the writers for the Cumberland Valley Railroad Company and used by that company in the various ways of calling attention to the desirability of its route. This model is based partly on actual survey and partly on sketch topography. The horizontal scale is ,%, the vertical 1/19,200 of

Jan 1, 1888

By C. B. Post, D. G. Schoffstall

A determinatioil of the hydrogen content of molten steel by means of the Vacuum-extraction method, as reported here, consists in first casting a sample of the bath in a bomb, so that the gases evolved during solidification are trapped for analysis. A portion of the cast steel sample is then prepared and heated at a temperature of 600" to 800°C. under high vacuum, and the gaser given off during this vacuum extraction (which are shown to be hydrogen), are collected and measured. Analysis of the gases evolved on solidification and the gases in the solid sample enables an accurate determination of hydrogen in the molten steel. Fig. I shows the bomb and accessories that have been found suitable for trapping the gases evolved on solidification. The bomb is made of scamless steel pipe, approximately 7 in. long by 136 in. i.d., and welded at the bottom. An ordinary pipe cap has a vacuuni-type metal stopcock threaded and brazed in its upper end. This pipe cap fits onto the bomb by means of machined threads. A flange is brazed to the pipe at the point where the cap starts to tighten up, and a rubber gasket is placed between the flange and cap. Heavy vacuum grease is used between the flange and gasket and the gasket and cap. The weight of the complete bomb and it? interval volume is known before the sample is cast. In practice, a sample of about 400 grams of steel is poured into the bomb, the funnel quickly swung out of the way, the bomb cap spun down the threads and tightened against the gasket, and the bomb set in a pail of water to keep the gasket and vacuum grease cool. It is estimated that at least 80 per cent 01 the gases evolved from the liquid sample during solidification are trapped in the bomb."

Jan 1, 1945

By Sydney H. Loram

The following notes have been compiled more for the reason that the district is little known to the outside world for its gold production, than for the hope of giving valuable information. The district of Canutillo lies about 15 miles south of the city of Freirina (1at. 28' 50' S. long. 70" 75' W.), and contains nine principal veins, all within a radius of a mile; 50 or more claims have been located on these veins, and this paper refers chiefly to those belonging to the Anglo-Chilean Exploration Go., Ltd., on which the greater part of the development work has been done. In all probability the mines were first worked by the Incas, who, under Tupac Yupangui, captured the country as far south as the Mauli river, between the years 1430 and 1470, and imposed a yearly tribut,e of gold and copper, which was forwarded by carriers on foot to Cuzco, the Inca capital in Peru. In the year 1535, soon after the time of the Spanish conquest, the stories of these consignments, together with those of supposed precious stones, led Diego de Almargro with a band of 400 soldiers to explore as far south as the Incas had gone, in the hope of finding the source of the precious metal, which he believed to have come from some definite point instead of being, as was afterwards proved, the collection of innumerable districts scattered over the entire length of the country. The method of winning the gold used by the Incas or by the natives whom they forced to work seems to have consisted in removing the ore by hard-wood wedges driven by stone-hammers, while a human shoulder-blade worn along its rounded edge, found in one of the mines, had evidently done duty to its second owner as a scraper or shovel. The mining was done by steep inclined workings sunk on the lodes at about 40" from the horizontal, the direction being reversed every 10 or

Jan 1, 1905

By John Norton

IN recent years, the damping capacity of metals has come to be recognized as an important index of certain types of structural change. In a number of instances, this property has proved to be particularly sensitive, but insufficient work has been done to permit a general inter-pretation. There is considerable question at the present time as to just what factors are responsible for the internal dissipation of energy when a metal is carried through a cycle of stress, and these factors must be ascertained if the value of the damping method as a metallurgical tool is to be determined. Since internal stresses are among the chief causes of dissipation of internal energy, or damping capacity, it was thought that a study of the changes in damping during the recovery and recrystalliza-tion of a cold-worked metal might throw some light upon the subject, particularly if the damping changes were correlated with other properties that are better understood. Probably more work has been done on the recrystallization phenomena of alpha brass than on any other metal, so this was chosen as the material for the present investigation. Damping measurements on brass have been made by Förster and Köster.1 They showed that the annealing of a brass that had been cold-drawn to 50 per cent reduction produced a rapid fall in the damping, a flat minimum occurring at approximately the temperature of recrystal-lization. The damping remained at a low value until grain growth was well under way and then it increased rapidly with increasing grain size. Köster and Rosenthal2 continued the work in greater detail. They pointed out that the damping decrease does not correspond to the hard-ness drop but occurs at a lower temperature, suggesting that the relief or redistribution of internal stresses has a large effect while the actual recrystallization effect is small. They also show the increase in damping at the higher annealing temperatures. Their curves are reproduced in Fig. 1.

Jan 1, 1940

By D. F. Stein

In spite of the apparent usefulness of autoradiography in demonstrating segregation, it has had very limited success in demonstrating grain boundary segregation. Because of this limited success, a model system amenable to mathematical analysis was devised to determine which variables in the experiment are most important. As a result of these calculations, it was concluded that autoradiograPhy is a rather insensitive technique to measure grain boundary segregation. The range (energies) of the emitted particles (ß and a) must be low, and the concentration of the radioactive speczes at the grain boundary must be (in general) two or three orders of magnitude greater than the concentration within the grain. Because of these very restricted conditions , the limited success of the technzque is not surprising. In spite of the apparent usefulness of autoradiography in demonstrating segregation, it has had very limited success in demonstrating grain boundary segregation. Sulfur segregation in iron1 and possibly polonium segregation in Pb-5 pct B1 2 alloys are the only autoradi-ography experiments that have demonstrated segregation to grain boundaries in metals without the formation of a second phase. Segregation to a boundary without the formation of a second phase is often called Gibbs' absorption and is discussed by McLean in Chapter 5 of Ref. 10. There are several394 experiments showing grain boundary diffusion of a radioisotope, but this type experiment is not representative of equilibrium between the concentration of an element at a grain boundary and that in bulk, so it will not be discussed in this paper. In an attempt to determine if temper embrittle ment of low-alloy steels was associated with segregation of antimony to grain boundaries, a program to use auto-radiography (using Sb-125) was initiated. Even though other measurements strongly suggest that segregation is occurring during embrittlement, no evidence of grain boundary segregation was observed in the auto-radiography experiments. An attempt was also made to detect segregation of carbon (using C-14) to grain boundaries in iron during slow cooling. There is again strong indirect evidence7 that segregation occurs during such a treatment, but the autoradiography experiment gave no evidence of such segregation. Because of the failure of these experiments and the general lack of success by our metallographic unit in measuring grain boundary segregation using autoradi-ography, a model system amenable to mathematical analysis was devised to determine which variables in the experiment are most important. MODEL SYSTEM The model system is illustrated in Figs. 1 and 2. It is a semi-infinite bicrystal with a single grain boundary perpendicular to the top face. The width of the grain boundary, W, is defined as the region to which segregation has occurred and it is assumed that this region is of constant composition. The assumption of an infinite dimension is for mathematical reasons but the results of such an analysis (as will be demonstrated later) are valid for even very small specimens. It also is assumed that the measurement is not limited by means of detecting the radiation (photographic emulsions, counters, and so forth) but that the means of detecting radiation is linearly sensitive to the radiation and has infinite resolving power. The distance y is the perpendicular distance from the center of the grain boundary to the point at which the background radiation is measured and x is the integration variable. CALCULATION FOR BETA PARTICLES Two values of the intensity of radiation will be calculated, the intensity at the center of the grain boundary and the intensity far from the grain boundary. The radiation at the center of the grain boundary can be calculated in the following way. Assume a grain boundary of width W having a uniform concentration equal to Cgb + Cb where CGb is the excess concentration of the element under consideration at the grain boundary and Cb is the bulk concentration. The intensity of radiation, IgB, at the center of the grain boundary, is a consequence of the amount of radioactive material, decay rate, absorption, and geometrical factors which can be represented mathematically by the following expression:

Jan 1, 1968

By M. M. Mebta, G. W. Dean, W. H. Somerton

With the advent of underground heating operations, interest has developed in the alteration of rock properties by high-temperature treatment. In the present work a number of sandstones were heated to temperatures in the range of 400°C to 800°C under both atmospheric and simulated reservoir pressures. Pertneabilities increased by at least 50 per cent and sonic velocities and breaking strerlgths decreased by an equivalent amount. Differential thermal expansion and other reactions of constituent min-era1 grains are the causes of these alterations. INTRODUCTION In the underground combustion of petroleum reservoirs, temperatures of the order of 600C are reported to have been reached in the combustion zone.' At this temperature rocks are subject to extensive thermal alteration. Temperatures of this magnitude and higher may also occur in subsurface formations when subjected to bottom-hole heating, thermal drilling operations, and underground nuclear explosions. Temperatures of this magnitude might also be generated by conventional rock drilling methods at points of bit-tooth contact. In earlier work, the permanent deformation of rocks resulting from heating was reported. Major structural damage of rocks occurs due to differential thermal expansion of mineral constituents. A number of mineral alterations including crystal inversions, loss of water of crystallization and dissociation, may also contribute to changes in physical structure and properties of rock. In the present work, samples of three typical sandstones were heated to several temperatures up to a maximum of 800C and then allowed to cool to room temperature. Heating was done under both atmospheric pressure and simulated reservoir pressure conditions. Physical properties of the samples were measured before and after heating and comparisons made. Measured properties included permeability, sonic velocity, breaking strength and fracture index. Changes in physical properties were compared to changes in mineralogical characteristics as determined by thin-section. X-ray diffraction and chemical tests. EQUIPMENT AND PROCEDURE Two outcrop sandstones (Bandera and Berea) and one sub-surface sandstone (St. Peter) were selected for the tests. These samples have a wide ranee in composition and physical properties as shown in Table 1. The first series of tests was made on 2-in. diameter by 5-in. long test specimens. Test specimens used in all later work were 3/4-in. diameter by 1 1/8-in. long, this being the specimen size required for heating at simulated reservoir pressures. After careful washing, the cores were oven dried at 100 ± 5C for a minimum of 24 hours before the tests were run. Test specimens were heated in an electric furnace at a constant rate of temperature increase of 3C per minute. When maximum temperature of the run was reached, the sample was allowed to soak for one hour. The furnace was then cooled to room temperature at the same rate of 3C per minute. The entire heating operation was designed for reproducibility without subjecting the test specimens to excessive thermal shock. For samples heated under simulated reservoir pressures, a pressure cell designed by Dean was used (Fig. 1).3 The core sample was inserted into a thin-walled (0.006 to 0.01-in.) copper cup which was then mounted in a high-pressure cell. Provisions were made for the application of internal pore pressure as well as confining pressure. Tests showed that the thin-walled copper cup closed tightly around the core and satisfactorily transmitted confining pressure to the core. The core was heated by placing the entire cell into the electric furnace. The heating program was the same as that used in the atmospheric pressure runs: tempera-ture rise of 3C per minute to maximum temperature of the test, soaking at maximum temperature for one hour, and cooling at a rate of approximately 3C per minute. The cell was designed to withstand 5,000 psi at 1,000C. However, since it was considered likely that repeated heating and cooling would in time weaken the steel, 2,000 psi at 850C was set as a working limit. In the present series of tests, the pore pressure was held constant at 750 psi and the confining pressure at 1.500 psi. The pressure source was a high-pressure nitrogen tank. The two pressures were controlled manually but are accurate well within ± 50 psi.

Jan 1, 1966

By James E. Adler, Timothy C. Richmond

The Stillwater District is located in south central Montana approximately 75 miles southwest of Billings, the state's largest city. It lies along the northeast front of the Beartooth Mountains and is within the boundaries of the Custer and Galatin National Forests. The first white visitors in the district were the early trappers, who were soon followed by the prospectors. These early prospectors were drawn to the area by gold and silver discoveries at Cooke City in 1870 as well as by the large gossan formation in Verdigris Creek near the west bank of the Stillwater River and by several scattered smaller gossan exposures throughout the area. The first patented mining claims were recorded in September, 1886.

Jan 3, 1974

By B. F. Oliver, F. Garofalo

Gas-metal heterogeneous reactions and zone-lrelting were sinultarneously employed to produce several high-purity irons with low interstitial contents in a levitating- zone melter. Successive zone-tneltitzg pusses were made in carious sequences of atmospheves which included prepuvified tank hy-drogeta, water vapor hydrogen, palladiuril-purified hydrogen, and vacuunm of 2 x 10-6 Torr. Different irons ranging in purity from 99.89 to 99.996 pct with residual curbon contents of 17, 8 to 10, and 3 to 5 ppm have been Drepared. No measuvable gradient in the residual carbon content was observed along the entire zone-melted length (6-10 in.) in I-ilz.-diameter bars. The absence of a carbon-concentration gradient in the solid indicates an apparent distvihution coefficient of 1, an unusual condition. Internal friction, solid-state extraction, and hot-hardness results indicate that the level of mobile carbon in a iron depends on the gas-metal heterogeneous reactions employed. Purification under an oxidizing atmosphere resulted in the immobilization of nearly all of the carbon present at leuels of 10 ppm or less. Continuation of purification in a reducing atmosphere veturued the carbon to a state of mobility which was aguin reversed by further purification in all oxidizing atmosphere. The immobilization of curbon at "vesidual levels " is believed to be associated with a strong interaction between carbon and oxygen atoms. frons with low carbon and nitrogen contetzts which did not exhibit a hot-hardness peak were produced after zone ynelting in vacuum. CARBON, nitrogen, and oxygen have strong and well-known effects on many properties of iron. These effects persist even at concentrations of 5 to 20 ppm. The intent of the present investigation was to establish procedures for the preparation of high-purity iron with concentrations of these elements in the range of 5 to 20 ppm and lower. The results reported here deal with the procedures employed to prepare high-purity iron, and with observations on the behavior of certain elements at "residual levels": particularly carbon. The details of the (levitating) zone melter in which the final purification steps are performed and the necessary control of the pertinent solidification variables have been described previously.1,2 MATERIALS AND PROCEDURES Commercial electrolytic iron was induction vacuum-melted and cast into 30-lb ingots. Melt additions and ingot analyses for carbon, oxygen, and nitrogen are noted in Table I. All ingots were melted in stabilized zirconia crucibles conditioned with one iron wash heat. Middle sections of the ingots were forged to 1-1/4-in. rounds, machined to 1-in.-diameter bars, then cut to 36-in. lengths. The zone-melting operations were performed on six iron bars (A to F) at a freezing velocity of 2 in. per hr with the freezing interface rotating2 at 200, 300, or 400 rpm. Liquid zones were passed through the bars in various sequences of atmospheres, Table 11, including prepurified tank H2, palladium-purified Hz, wet H2, and system vacuum of 2 x 1018 Torr. Wet-Hz atmospheres were obtained by bubbling palladium-purified Hz through water exhibiting a resistance of 3 megohms. This water was heated with a platinum-immersion heater and was degassed prior to use. Zone melting in a wet-HZ atmosphere resulted in oxidation of the elements which are oxi-dizable with respect to iron. Fine oxide particles were observed on the surface of the liquid zone, and were encased in the bar surface with the passage of the molten zone. Between each zone pass, the surface of the bar was removed by filing and deep etching; this was continued until the oxide formation ceased. The filings were magnetically separated and the residues analyzed by optical spectroscopy. These were especially high in silicon and manganese. Samples were removed from the iron bars, with few exceptions, following each zone-melting operation. A 0.08-in.-thick disc was cut with an Al2O3 cut-off wheel at a point 1/2 in. above the beginning of freezing. Material from each disc was used for hot-hardness measurements, resistivity-ratio measurements, and carbon, nitrogen, and oxygen analyses. Analyses for most other elements were

Jan 1, 1965

By G. W. Thomas

A simplified mathematical model of underground conduction heating in a system of limited permeability is presented. The model applies to underground retorting of oil shale, or to reservoirs containing extremely heavy oils. We assume that heat is introduced at a constant rate into a horizontal fracture which communicates between wells. The radial temperature distribution along the fractured surface is approximated by a step-function. Heat transfer away from the fracture is assumed to be by vertical conduction, and all convection effects are neglected. The model also takes into account the possible temperature dependence of thermal conductivity. A general expression for calculating the growth of the step-function temperature distribution with time is derived. The use of this expression and solutions to the one-dimensional heat equation make it possible to construct isotherms. Expressions for calculating .oil recovery, well spacing and heat efficiency are also given. An example calculation is presented for the conduction heating process in oil shale. Finally, the effect of the heat transfer coefficient between the gas and the fracture boundaries is investigated. INTRODUCTION Thermal recovery processes of oil recovery fall into the four general areas of hot fluid injection, forward combustion, reverse combustion and conduction heating. The first three of* these processes have been rather extensively studied in the past decade from both the experimental and theoretical points of view. As a result, it is possible to make reasonable engineering predictions and analyses of these processes. Little attention has been devoted, however, to the conduction heating process other than to note its possible utility.I To a certain extent, conduction heating cannot be divorced from the other regimes cited above, insofar as these provide the source of heat energy. In the conduction heating process, heat is introduced (either by combustion in the forward or reverse mode or by hot fluid injection) into a small fraction of the total reservoir thickness. This fraction may be either a streak of high permeability or an interwell fracture. Heat penetrates by conduction into the adjacent, less permeable regions of the oil-bearing rock, where the direction of conduction is essentially perpendicular to the streak or fracture. The heated product then drains by gravity or is gas driven to production wells. Conduction heating is probably most applicable to systems containing immobile bitumens such as tar sands and oil shale deposits and perhaps to low-permeability reservoirs containing highly viscous crudes. The mechanism also acts in combination with other thermal processes where fingering or overriding of a bed occurs. It seems probable that in at least one field test, conduction heating of this type was very influential.2 In this presentation we give a first approximation to some of the quantitative aspects of conduction heating. Marx and Langenheim3 treated a similar problem where they focused attention upon the injection interval, which spanned the total reservoir thickness. In their model, conduction heat losses to the bounding media imposed a practical limit on the calculated heated area. In the present study, however, we shall confine the injection interval to a small fraction of the reservoir thickness and assume it has no heat capacity. We therefore direct our attention to regions outside the injection interval into which the conduction of heat is beneficial. In particular, we will endeavor to locate specific isotherms in the media bounding the injection interval. Furthermore, we will construct our model to allow the thermal conductivity to vary arbitrarily with temperature. Thus the model will be applicable to underground retorting of shale where variations in thermal conductivity may be important. THEORY We consider the rock matrix to have no or, at best, a very limited permeability; consequently a

Jan 1, 1965

By W. V. Green

The creep-rupture behavior of commercial powder-metallurgy tungsten rod is reported for temperatures of 2250°, 2500°, 2700°, and 2800°C, stresses up to 7000 psi, and times up to 4 hr. The temperature dependence and the stress dependence of creep rates are evaluated. Rupture time is fitted to the Larson-Miller parameter and compared to lower-temperature and higher stress results reported by pugh.4 THE tensile strength of single-crystal wire1 and of polycrystalline wire2 have been measured by Goucher. More recently Bechtold3 and pugh4 have studied the mechanical properties of tungsten rod between room temperature and 1200°C. Since tungsten has the highest melting point of all metals, it should retain useful strength to very high temperatures, and should find many applications in missiles, rockets, and so forth. Therefore, the mechanical usefulness of polycrystalline tungsten rod was investigated in the 2250" to 2800°C temperature range by short-time creep-rupture tests. MATERIALS TESTED Creep specimens were machined from 1/2-in. round commercial tungsten rod which was manufactured from powder by cold pressing, sintering, and hot swaging. Purity reported by the vendor was 99.95 pct W. Spectrochemical analyses showed "traces" (less than 0.01 pct) of silicon, iron, and titanium, and "faint traces" (less than 0.001 pct) of calcium and manganese. Carbon content was 30 ppm and nitrogen content was 70 to 110 ppm. No oxygen analysis was obtained. Room-temperature stress-strain tests on the as-received tungsten gave badly scattered results. Threaded end specimens broke at the threads. When these specimens were retested using shoulder grips, the specimens broke at the shoulders. No fractures occurred in the gage lengths. The fracture stresses were: 127,000; 137,000; and 154,000 psi for three specimens which fractured at the shoulders. The microstructure of the as-received tungsten rod is shown in Fig. 1. SPECIMENS USED Fig. 2 shows the two types of creep specimens tested. The threaded-end type specimen, which was used in most tests, had a 3/4-in. gage length and 1/4-in. gage diam. The cone-end specimen, which was used primarily to investigate the effects of a smaller gage diameter and the practicability of the modified grips and specimen, had a 3/4-in. gage length and a 1/8-in. gage diam. In both cases, the gage length terminated at 0.005-in. high shoulders which served as fiducial marks for optical strain measurements. Surface finish on the gage length was 16 µ-in. rms. Creep rates and rupture times were not significantly different for the two types of specimens and were not affected by electropolishing the specimens before testing. TESTING PROCEDURE The constant-load creep-testing machine used has been described by Smith, Olson, and Brown.5 In it the specimen is held vertically by grips of similar material and on the axis of a cylindrical tungsten or tantalum heater-tube. The specimen is loaded by means of the specimen grips, a pull rod (which is sealed to the chamber lid by a vacuum-tight bellows), a mechanical lever system, and hanging dead weights. Both specimen and grips are heated by radiation from the heater-tube, which is heated by its own electrical resistance. An optical system views the incandescent specimen through slits in the radiation shielding and heater-tube. The optical system projects an enlarged image of the specimen gage length on a ground-glass screen. Periodic gage-length measurements are made on this image with two cathetometers. Thorium oxide coatings on the specimen threads or conical end surfaces completely prevented diffusion-welding of specimens to grips, and were used

Jan 1, 1960

By H. M. Strong

Nickel and carbon form a metastable nickel-nickel carbide eutectic system which was ohsen)able by freezing latent-heat arvests at pressures 210 khars. The eutectic freezing temperature Is pressure had a slope of -0.9°Cper kbar. At 50 khars, the nickel-nickel carbide eutectic was at 1297° * 5°C and 0.34 mole fraction Ni3C. The composition of the eutectic increased at an initial rate of 0.004 mol fraction per kbar. The carbon content of the a phase also increased with pressure. Seveval illustrations of nickel carbide microstruc-tures are given and data on the lattice expansion of nickel in terms of carbon content are included. IRON, cobalt, and nickel form a variety of carbides with compositions varying between MeC and MC. Of the three, the carbides of iron are most easily recovered. The nickel carbides are so unstable at temperatures above 900°C that their occurrence in Ni-C alloys is unusual. Under sufficient pressure, however, the temperature range for the stability of the ferrous metal carbides is likely to be increased, or their decomposition suppressed (e.g., see Hilliard' on FesC), providing an opportunity to study the unstable carbides more closely. This was found to be true for nickel carbide which, under pressure, formed a eutectic with nickel. This paper describes the conditions of formation of nickel-nickel carbide eutectic compositions and their subsequent recovery. Despite the comparative instability of the nickel carbides, something is already known about them through various chemical reactions at temperatures not exceeding a few hundred degrees, and from their recovery by the very rapid quenching of molten Ni-C alloys from temperatures of about 1450°C or above. At least four carbides of nickel have been reported: A discussion of the state of knowledge about Ni3C is given by ansen.' The studies of Morrogh and williams7 who obtained Widmanstatten nickel carbide structures and of sidorenko8 who first obtained nickel carbide eutectic structures are also of interest. Sidorenko used short heating times for molten nickel in a graphite crucible followed by very rapid quenching to obtain the eutectic structures. Long heating times produced only the nickel-graphite eutectic probably due to the presence of graphite crystals in the melt which nucleated graphite crystallization. According to the early work summarized by anssen,' nickel carbide may form at temperatures far above the melting point and may be recovered by very rapid quenching. More recently, Giardini and Tydings, working on diamond synthesis, found evidence for "free nickel carbide'' in high-pressure reactions carried to temperatures far in excess of the limit for diamond growth, followed by rapid thermal quench. They stated that nickel carbide was not found in association with diamond growth. In the present work, observations were made on the melting and solidification temperatures of Ni-C alloys as a function of composition, temperature, and pressure. The nickel-nickel carbide eutectic was found at pressures above 10 kbar and its variation with pressure followed up to 60 kbar. Nickel-nickel carbide microstructures were recovered by quenching under pressure from temperatures of about 1400°C and higher. The formation of nickel carbide structures under ordinary diamond-growing conditions was usually observed but the role of carbide formation as an intermediate step in diamond growth needs more study. EXPERIMENTAL METHODS The melting and solidification temperatures of various nickel-graphite compositions were observed by latent-heat arrests in the sample holder illustrated in Fig. 1. The samples were composed of mixtures of carbonyl nickel powder and National Carbon Co.'s SP-1 graphite packed to densities of about 6.4 g per cu cm. They were contained within

Jan 1, 1965

By H. D. Outmans

The mechanics of filtration are described by a theoretical-empirical nonlinear diffusion equation which, under certain circumstances, may,be linearized and then solved explicitly. For filtration under static conditions linearization leads to a boundary value problem analogous to a heat flow problem with a known explicit solution. The corresponding solution for static filtration is compared with published experimental data. Under dynamic conditions filtration takes place in three successive stages. During each of these the rate of filtration and/or the thickness of the filter cake are different functions of the filtration time. The proposed mechanism explains the observed high resistance of dynamically deposited filter cakes against erosion and also the connection between filtration rate and viscosity of the drilling fluid. Several of the quantities governing dynamic filtration have no counterpart in the static filtration mechanism. The static filtration rate is, therefore, not a reliable measure for the dynamic rate and vice versa. INTRODUCTION Filtration under simulated borehole conditions, i.e.. either from a static suspension or from a suspension flowing parallel to the filter cake (dynamic filtration), has been the subject of several laboratory studies.1-7 This experimental and theoretical work showed that many aspects of the filtration mechanism cannot be explained by an elementary filtration theory based on the assumption that the filter cake is incompressible. For a more satisfactory theory compressibility should be taken into account. This has been done. at least to some extent, in the filtration theory developed for the chemical industry. Surveying the literature (see Ref. 8 for a bibliography) it becomes apparent that, although several properties of filter cakes deposited from many different suspensions have been measured, including compressibility, the filtration equations are essentially empirical in nature. No attempt has been made, for instance, to develop filtration theory along the lines of consolidation theory.12 This theory, upon which a highly successful development in soil mechanics rests, would appear to be an excellent starting point for a filtration theory since the compressibility concept is an essential part of it. As we will use this theory in the following development it is well to state the four assumptions on which it is based: 1. The fluid flow through a compressible porous medium is governed by Darcy's law. 2. The rate of change in fluid content of an element of the porous medium is proportional to the rate of change of solid pressure between the particles. 3. The solid particles are incompressible within the range of pressures considered. 4. The total pressure on a surface normal to the line of flow is equal to the sum of the fluid pressure and the pressure between the particles (solid pressure) at that surface. To calculate the rate of filtration and other quantities of interest it is necessary to know the filter cake compressibility and the permeability as a function of the solid pressure. It has not been possible to calculate these functions from theoretical considerations and they will therefore be introduced in this paper as empirical expressions. Both are determined in a compression cell where the cake is subjected to a mechanical load. Permeability and compressibility are measured after the solid pressure has stabilized, i.e., after the excess fluid pressure has been dissipated and the uniform pressure is transmitted entirely by the solids. The permeability and compressibility thus determined are not the same as during filtration in the borehole, under either static or dynamic conditions, because then, due to frictional drag, the solid pressure and hence also the permeability and compressibility vary along a line normal to the direction of the mean flow and can only be defined locally. DERIVATION OF THE FILTRATION EQUATION FOR COMPRESSIBLE FILTER CAKES As the filter cake in the borehole is thin compared to the radius of the hole the filtration may be considered as linear. Taking the x-axis normal to the wall, with its origin at the formation, we have, according to Darcy's law,

By Frank R. Milliken, Robert Goodwin

In September 1937, the Ohio Copper Co. inaugurated the treatment of its copper-bearing mill tailings at Lark, Utah. These tailings had been accumulated during the regular operation of the Ohio Copper mine and mill over the period 1907 to 1919. Gravity concentration had been employed except for a comparatively short period in 1919, when flotation was used. The ore milled during that period assayed about I per cent Cu. The chief copper mineral, chalcocite, was disseminated in a shattered quartzite, mainly along fracture or cleavage planes. The quartzite gangue was extremely hard and grinding to liberation resulted in excessive sliming of the "sooty" chalcocite, with consequent high tailings losses. Recovery on the seven million tons treated was probably less than 60 per cent of the total copper content. As early as 1918, attempts had been made to sample the dump. In 1928, a complete sampling program was undertaken. The sampling consisted of seventy-four 5-in. post auger holes drilled to the full depth of the dump at regular intervals of 250 ft. Each 10-ft. portion thereof comprised a sample for analysis. Each sample was screened, rolled, divided into three parts, dried and assayed. The reject was retained for testing purposes. From the depth of the auger holes a contour map of the dump was plotted, Fig. I, which gives percentages of tonnage and copper content. The tonnage within the limit of the drill holes was estimated at about five million tons with an average content of 0.42 per cent Cu, 31 per cent of which (0.13 per cent) was acid-soluble. A screen analysis of the composite dump sample is shown in Table I. Flotation tests by several companies and individuals were then made, the results of which ranged from 62 to 74 per cent recovery. On the basis of these, a 200-ton pilot plant employing straight flotation was built and operated for a few months. Operation of this plant was unsuccessful, as no provision had been made to handle the copper-bearing solutions resulting from the water-soluble copper, a point that was overlooked in the laboratory test work. Attempts to decant the copper-bearing solution for precipitation in the usual manner ahead of flotation were not satisfactory because of low water recovery (owing to poor settling characteristics of the pulp) and contamination of the copper precipitate with unsettled slime. Low copper prices in 1931 necessitated the termination of testing. With the stimulus of higher copper prices in 1937, a review was made of metallurgical

Jan 1, 1943

By Michael B. Bever, Carl F. Floe

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

By Carl F. Floe, Michael B. Bever

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

By E. H. Rose

THE present symposium on flotation machines provides a unique opportunity for group reappraisal of standard or habitual viewpoints. A symposium is by definition a trading post for observations that might prove complementary when put together, thus leading to useful thoughts that might not have been evident from the original observations individually. The present paper, pertaining to power consumption in flotation, is deliberately an experiment of that kind. Data were solicited from the operating superintendents of several of the major flotation plants on this continent. The information received, covering a total of 14 separate operations in seven plants, has been collated in terms of power intensity; that is, the total power input per cubic foot of cell volume. This departs somewhat from the conventional expression of power per ton of ore treated, though the latter figure is also given for the plants concerned. Because of wartime restrictions, particularly in Canada, identifying names of plants and machines are withheld. Not as a firm conclusion, but as a tender for symposium discussion, the following points are made: I. That flotation is a power operation in much the same sense as ball milling. 2. That contact time is the complement of power intensity and may be decreased as the latter is increased. 3. That a decrease in flotation power per ton of ore can result from an increase in power intensity. ANALOGY WITH GRINDING In grinding, it has become axiomatic that the more the power put into a given operation, the greater the work performance. The analogous view is now proposed that the effectiveness of any flotation operation will be related to the mechanical energy usefully applied to that operation. Under this view, each increment of properly directed input energy should give either an increase in unit tonnage or an improvement in the metallurgical separation (concentrate grade or tailing grade), until either the theoretical limit imposed by mineral constitution or surface condition is reached, or until further increments of power become uneconomic under the law of diminishing returns. Thus, as in grinding, there are two forms of output that greater power input or improved utilization of power can produce. As for the law of diminishing returns, lower unit cost of power through improved generating efficiency in the past decade has pushed the limit back. Over and above this, however, there is strong indication in the operationg data herein presented that higher power intensity results in an actual economy of over-all power consumption. Like crushing and grinding, flotation accomplishes a rupture of the forces of molecular attraction, by taking particles from the common environment and placing them in the two separate environments of

Jan 1, 1944

By Frederic Lahee

THE total production of crude oil in Texas during 1924 was said to be 133,613,985 bbl. as compared with 125,991,628 bbl. in 1923.1 Subtracting from these figures the yield of the Gulf Coast fields, there remains, for the other part. of Texas, a yield of 106,272,573 bbl. in 1924, as compared with 101,931,595 bbl. in 1923. This represents an increased, production of over 4,250,000 bbl. for all of Texas outside of the Gulf Coast or Salt Dome fields. Within this same region, in 1924, there were 3624 completions, of which 2352 were oil or oil and gas wells, 7 were gassers, and 1265 were dry holes. Thus, nearly 35 per cent. of the completions were dry holes. In 1923, there were 4134 completions, with 2853 oil or oil and gas wells, 2 gas wells, and 1279, or 31 per cent. of the total, dry holes. Outside of the Gulf Coast region, six major pools were discovered and developed in 1924.; two pools, previously discovered, were extended far beyond their limits at the end of 1923, and many smaller pools were opened. The major pools were the Big Lake field, in Reagan Co., the New Richland field, in Navarro Co., the Harmel, Carey, and Ragle pools, in south Archer County, and the Wortham field, in Freestone and Limestone Counties. Fields that were notably extended were the Panhandle producing area and the Luling field. Many wildcat wells have been drilled; most -of these were failures, but several opened .pools and several have had sufficiently favorable results to. lead to further drilling. The activity of the operators in searching for new production was very intense during 1924, and indications point to as feverish a campaign during the coming year. This will be stimulated by rising prices for crude oil. There are good reasons for believing that new pools will be discovered along the Mexia fault zone, in Archer, Young, Baylor, and Throckmorton Counties, in the great central region of Texas where we now have the Mitchell County and Reagan County pools, and very likely in the eastern Red River Counties including Cooke and Grayson. On the other hand, with the opening of the year, there is no new big pool in sight. An outstanding feature of the production end of the business is the increasing reliance placed on geological work and geological recommendations. Not in five or six years has there been such a demand for first-class geologists.

Jan 3, 1925

By Alfonso Rizo-Patrón, A. M. Gaudin

PREVIOUS studies of activation in flotation have directed attention to the action of the activator on the mineral to be floated rather than to the relationship of the activator to the collector. The latter phase of the problem, however, seems to have definite scientific, if not also practical, interest. In the investigation reported in this paper, experiments were carried out, largely with quartz as subject, barium as activator, and oleate as collector. The results obtained indicate that a I : I ratio of collector ion to activator ion gives optimum results, and that a 2:I ratio almost fails to achieve activation and flotation. Yet, a 2:I ratio would have been expected on stoichiometric grounds, had the coating been a normal salt of the activator ion with the collector ion, since barium is a divalent cation and oleate a monovalent anion. To interpret and rationalize the observations, considerations of the crystal chemistry of quartz are helpful. The point of view to which these considerations lead may be of general applicability to systems involving suspensions of solids in liquids; they confirm that an adsorbed coating is inescapable. APPARATUS AND SUPPLIES The experimental work consisted in barium-ion abstraction tests, hydrogen-ion and hydroxyl-ion abstraction tests, flotation tests, and determinations of the surface of the crushed quartz. The flotation machine was built according to the design of D. W. McGlashan.* It consists of a drill press in which the bit has been replaced by a stainless-steel impellor surrounding a stainless-steel stator, as in the Fagergren laboratory machine. The air intake is controlled by a valve, and the cell consists of a beaker. The quartz was obtained from vein quartz stored in large chunks. It was first crushed to 20 mesh, then sized on a 28-mesh screen. The 20 to 28-mesh size alone was retained for use. This size was freed of coarse iron by passage through a Ball Norton magnetic separator, bleached with boiling hydrochloric acid to remove residual abraded iron, washed with distilled water until the washings were thoroughly free of ferrous, ferric, and excess hydrogen ion, and stored in covered Pyrex beakers under water until used. The barium was used as barium chloride, Baker's analyzed C. P. The oleate was used as sodium oleate. It was prepared from sodium hydroxide, Baker's analyzed C. P., and oleic acid purified by R. R. de Arellano3 in the laboratories at the Massachusetts Institute of Technology. The purification procedure was elaborated from the recent researches of Brown and Shinowara.2 It consisted in: (I) saponification of olive oil with potassium

Jan 1, 1942

By Robert Goodwin, Frank R. Milliken

In September 1937, the Ohio Copper Co. inaugurated the treatment of its copper-bearing mill tailings at Lark, Utah. These tailings had been accumulated during the regular operation of the Ohio Copper mine and mill over the period 1907 to 1919. Gravity concentration had been employed except for a comparatively short period in 1919, when flotation was used. The ore milled during that period assayed about I per cent Cu. The chief copper mineral, chalcocite, was disseminated in a shattered quartzite, mainly along fracture or cleavage planes. The quartzite gangue was extremely hard and grinding to liberation resulted in excessive sliming of the "sooty" chalcocite, with consequent high tailings losses. Recovery on the seven million tons treated was probably less than 60 per cent of the total copper content. As early as 1918, attempts had been made to sample the dump. In 1928, a complete sampling program was undertaken. The sampling consisted of seventy-four 5-in. post auger holes drilled to the full depth of the dump at regular intervals of 250 ft. Each 10-ft. portion thereof comprised a sample for analysis. Each sample was screened, rolled, divided into three parts, dried and assayed. The reject was retained for testing purposes. From the depth of the auger holes a contour map of the dump was plotted, Fig. I, which gives percentages of tonnage and copper content. The tonnage within the limit of the drill holes was estimated at about five million tons with an average content of 0.42 per cent Cu, 31 per cent of which (0.13 per cent) was acid-soluble. A screen analysis of the composite dump sample is shown in Table I. Flotation tests by several companies and individuals were then made, the results of which ranged from 62 to 74 per cent recovery. On the basis of these, a 200-ton pilot plant employing straight flotation was built and operated for a few months. Operation of this plant was unsuccessful, as no provision had been made to handle the copper-bearing solutions resulting from the water-soluble copper, a point that was overlooked in the laboratory test work. Attempts to decant the copper-bearing solution for precipitation in the usual manner ahead of flotation were not satisfactory because of low water recovery (owing to poor settling characteristics of the pulp) and contamination of the copper precipitate with unsettled slime. Low copper prices in 1931 necessitated the termination of testing. With the stimulus of higher copper prices in 1937, a review was made of metallurgical

Jan 1, 1943

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,',' 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