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By E. Bicknese, R. Clark

The mechanism and rate of reduction of FeO at conditions similar to those in the stack of a blast furnace have been determined for temperatures from 980" to 1165°C. Preliminary studies of the reduction of Fe2O3 with activated coconut charcoal in a static system (no flow of reducing gas) have shown that the CO2-CO ratio of the product gas depends upon the relative reactivities of the Fe2O3 and charcoal. In a systern with a "hot blast" of CO and Nz (simitar to dry bosh gas), synthetic FeO, and actiuated coconut charcoal, the rate of reduction was not sensitive to the flow of reducing gas, and the rate-controlling step alas the chemical reaction at the metal-oxide interface. Wherz solid carbon was not present, a critical flow rate of reducing- gas had to be met in order to prevent a lowering of the reduction rate. The effect of a less-reactive carbon (blast-jurnace coke) and of a "natural" FeO on the mechanistn and rate, and the mininum amount of carbon necessary in the charge to tnaintain the reducing potential of the gas phase, have been determined. THE importance of iron oxide reduction processes has encouraged many studies of the process reaction kinetics. Despite this, the mechanism is not well-understood and three main theories have evolved, which can be stated as follows: A) the rate-controlling step is diffusion, either gaseous diffusion of the reductant or product gas through a porous solid,' or solid-state diffusion of iron and oxygen atoms through the so1id.2 B) The slow step is diffusion of reducing gas through a stagnant boundary layer. C) The reaction rate is controlled by the chemical reaction occurring at the metal-oxide interface and is proportional to the area of this interface.3 By increasing the velocity of the reducing gas to a flow rate beyond which no increase in the reduction rate is observed, critical flow rate, it may be possible to eliminate B as the slow step. However, as warnere points out, the establishment of a critical flow rate may only assure that the reaction is not limited by a reduction in the reducing potential of the gas and that B may still be the rate-determining step. Edstrom and Bitsianes and Seth and Ross8 show that A and C may both be correct for the reduction of the same oxide, depending upon the stage of the reduction, and that the relative importance of the two mechanisms varies with the porosity of the oxide. Themelis9 has derived expressions which express A, B, and C in terms of the fraction reduction, Rx, of a spherical particle. Thus, in the case of A a plot of In (1 - Rx) vs time must be linear and the time to reach a given reduction is proportional to the square of the particle diameter. For B a plot of (1 - Rx) vs must be linear and the time to reach a given reduction is proportional to the square of the diameter. For C a plot of 1 - (1 - RX)1/3 vs f must be linear and the time to reach a given degree of reduction should be proportional to the diameter. In the case of mixad controlled reactions, none of the plots are linear over their entire length. The results of previous studies, in which the rates of gaseous reduction of iron oxide were measured in the absence of carbon, may not correspond to blastfurnace practice because they ignore the effects of the Boudouard reaction. CO2 +C — 2CO The presence of carbon may alter the mechanism or the rate of iron oxide reduction through an enrichment of the gas phase by Eq. [1]. In this case, the presence of and reactivity of carbon become important. If the Boudouard reaction has no effect on the rate of reduction, the reducing gas could be supplied by some means other than the gasification of carbon at the tuyeres and carbon could, theoretically, be eliminated from the burden. Preliminary studies of the reduction of Fe2O3 with activated coconut charcoal were made to determine if the reactivity (surface area) of the Fe2O3 had any effect on the product gas composition. Two size fractions of Fe2O3 were reduced with charcoal in a static system (no flow of reducing gas). In each case the charcoal was -100 + 325 mesh and was 25 pct of the total charge. One fraction of the reagent-grade Fe2O3 was submicron in diameter. The other fraction was -100 + 200 mesh and was prepared from the former by compacting, sintering at 1300°C, crushing, and screening. In each experiment, the reaction vessel was filled with a mixture of CO and CO, which would be in equilibrium with FeO and iron at the reaction temperature. A furnace was heated to the desired temperature, the vessel was placed in the furnace, and the gaseous products of the reaction were collected and analyzed. The results of these experiments, Fig. 1, show that the gas phase associated with the submicron oxide is more oxidizing than that with the -100 + 200 mesh oxide. Therefore, in a static system, the relative rates of the reduction reaction and the gasification of carbon depend upon the reactivities of the Fe2O3 and charcoal. The reduction of FeO to iron is the most important reaction occurring in the blast furnace and is probably the slowest of the several reduction steps. The mechanism and rate of reduction of FeO in a system containing carbon and a flow of dry bosh gas have been studied. TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AlME

Jan 1, 1967

By N. S. Stoloff, M. Gensamer

The effects of temperature, grain size, and magnesium content on the strength and ductility of cadmium were studied in the range -269° to 23 °C. A sharp drop in ductility between -140° and -190°C marked a transition in fracture mode from ductile shear to inter gvanular fracture. The addition of up to 15.35 wt pct Mg in solid solution raised the transition temperature, and for two compositions produced basal cleavages. The relatively high ductility of unalloyed cadmium at cryogenic temperatures is attributed to temperature independence of the yield stress and the absence of dislocation locking. ALTHOUGH numerous studies have been made of the mechanical properties of cadmium single crystals,1-5 no comprehensive investigation of deformation and fracture in polycrystalline cadmium has been carried out. This investigation was initiated to determine the mechanisms of deformation and fracture in polycrystalline cadmium, and to attempt to correlate these mechanisms with the behavior of other metals of hexagonal close-packed structure. A second objective of this work was to determine whether the slip systems and mode of fracture of polycrystalline cadmium could be altered by reduction of the axial ratio, which is 1.886, through alloying. Dorn and co-workers' have been able to induce prismatic slip in magnesium through alloying to reduce the axial ratio. Single crystals of cadmium are so highly ductile that glide strains of 400 pct are observed at room temperature, and 80 pct at -269°c.l Failure in every reported case is by necking down and shearing off of the crystal. Cleavage in cadmium single crystals has never been observed. Magnusson and aldwin reported a ductile to brittle transition for polycrystalline cadmium at about —160 C for specimens tested at a strain rate of 0.05 in. per in. per min in tension. However, even at -196° substantial ductility was retained. The transition temperature was strain rate dependent, impact loading at 19,000 in. per in. per min raising the transition temperature to about -85°C while leaving the low temperature ductility unchanged. No information was given on microstructures or fracture mode, nor were stress-strain characteristics reported. In the present investigation, tensile tests were carried out on polycrystalline cadmium and solid solution Cd-Mg alloys to determine flow stresses, work-hardening behavior, fracture strength, and fracture ductility. Variables employed included temperature, alloy content (and c/a ratio), and grain size.Some compression data also have been obtained for comparison purposes. I) EXPERIMENTAL PROCEDURES A) Polycrystalline Cadmium. Two purities of cadmium were employed in this investigation. Cadmium of 99.95 pct purity was supplied by Belmont Smelting and Refining Co. Cadmium of 99.99+ pct purity was supplied by American Smelting and Refining Co. Threaded cylindrical tensile specimens were machined to give approximately a 1/2 in. long straight gage section with a reduced diameter of about 0.110 in. Specimens were heat treated in evacuated pyrex capsules in the range 140" to 290°C to produce desired grain sizes. All specimens were polished in a solution containing 320 g Cr03 and 20 g NaS04 in 1000 cc of H20. Occasionally this solution caused staining of the specimen, in which case a further polish with a solution of one part HN03 and two parts H202 in two parts ethyl alcohol was employed.' Tensile testing was carried out on a screw-driven Instron machine, at a constant rate of crosshead movement, which for most tests was 0.01 in. per in. per min. Load vs time, and therefore load vs total strain, were recorded. Temperatures from -196" to -40°C were obtained by passing nitrogen gas through a copper coil immersed in liquid nitrogen, and then feeding the gas into a jacket around the specimen. Tests at -269°C were carried out in a helium cryostat, at a crosshead rate of 0.1 in. per in. per min, with specimens of 1 in. gage length. Compression specimens were tested in a jig similar to one designed by ilman. The jig was mounted on the under side of the Instron crosshead. Load was transmitted by means of a rod connected to a movable part of the jig at one end, and the load cell at the other end. A downward movement of the crosshead applied a compressive load to the specimen.

Jan 1, 1963

By E. J. Rapperport, M. F. Smith

A presentation of the W-Ru constitution diagram is given. Techniques utilized in the determination of phase boundary values include electron micro-probe analysis of two-phased alloys and diffusion couples, as well as normal metallographic and X-ray methods. The primary features of the diagram are: 1) a terminal solid solution of ruthenium in tungsten with a maximum solubility of 23 at. pct Ru at 2300°C; 2) a terminal solid solution of tungsten in ruthenium with a maximum solubility of 48 at. pct W at 2205°C; 3) a o phase of maximum breadth about 6 at. pct based on the composition W3Ru2 which forms peritectically from the melt at 2300°C, and which decomposes eutectoidally at 1667 °C to form a twigs ten and 0 ruthenium; 4) a eutectic at 45 at. pct Ru and 2205°C with the products being o plus ß ruthenium. THE W-Ru diagram has previously been studied only in a cursory fashion. Raub and alter' obtained a 1400°C isotherm in which they observed no intermediate phases, and on which they established the limits of solubility as 36.5 at. pct W in ruthenium and about 1.5 at. pct Ru in tungsten. In addition, Obrowski2 found a o phase forming peritectically from the melt and existing only above 1650°C. Below this temperature the phase was presumed to decompose eutectoidally. The present work finds the diagram as given in Fig. 1. I) EXPERIMENTAL PROCEDURE The materials used for alloy preparation in determining the W-Ru constitution diagram were 99.9 pct pure ruthenium powder supplied by Baker Chemical Co., and 99.9 pct pure tungsten powder from General Electric Co. Typical analyses of these elements are given in Table I. Initial alloys at 10 at. pct intervals were prepared from the metal powders by the following method. Powders sufficient for 25 g of the alloys were weighed out with an accuracy of 0.1 mg and blended mechanically. After blending, the powders were compacted, in a steel die, at approximately 30,000 psi. The compacts were sintered in an electric vacuum furnace in order to remove adsorbed gases and to achieve partial densification prior to arc-melting. Vacua of 10-4 mm Hg or less were maintained in sintering as the furnace temperature was raised to approximately 2000°C. Sintering times ranged from 10 to 20 hr. The sintered compacts were arc-melted under a protective atmosphere of purified helium. Melting was conducted on a water-cooled copper hearth, utilizing a nonconsumable tungsten electrode. In the melting process, each alloy was turned over and re-melted on opposite sides from four to six times to ensure complete melting and to eliminate gross in-homogeneities. The arc-melter used had a vacuum capability of 5 X 10-6 mm Hg, and a leak rate of about 20 -liters per hr. Chemical analysis techniques for refractory metal-platinum group metal combinations are not well-established; therefore, composition control and determination depended principally upon weight-loss observations and calculations. This consisted in weighing each alloy after sintering and after arc-melting, and calculating the maximum and minimum composition values, assuming the total weight losses to be first all tungsten, and then all ruthenium. Since composition uncertainty was directly related to weight loss, care was taken to minimize losses in handling, compacting, and melting. Prior to homogenization and equilibration the as-arc-melted alloys were analyzed in several

Jan 1, 1964

By T. S. West

Completion and production data presented for three wells in the Oakville area of Live Oak County, Texas, which were completed near the gas-oil or water-oil contact, indicate that coning may not be as prevalent a cause of failure in such cases as is commonly assumed. Failure in the cases discussed is indicated to be due instead to: (I) erosion of the formation, (2) flowing out of mud filter cake, or (3) failure of the cement. An open-hole gravel-pack type of completion procedure is proposed for preventing failures of this kind by preventing movement of all solid material in the space in which completion is made. Various combinations of layers of gravel, sand, and cement are utilized for this purpose. Experimental results and theoretical discussion as to the applicability of gravel pack completion are included. Introduction This paper is primarily a study of the reasons for failure of oil-well completions near the gas-oil or oil-water contact, and suggests a procedure for increasing the efficiency of this type of completion. The value of improvement in completion effectiveness near the gas or water zone is not confined, however, to wells of relatively thin oil columns. Thick oil columns become thin as depletion progresses. It would seem to follow that the minimum distance from the gas or water zone at which completion can be made in a new well indicates the limit to which depletion may be carried in a well having an oil column of any initial magnitude. Only four ways can be postulated in which high gas-oil or water-oil ratio can initially occur if the zone exposed for production is within the oil column: 1. Failure of the cementing material. 2. Vertical coning. 3. Failure along the boundary between the cement and the wall of the well. 4. Failure of the formation comprising the wall of the well. Cementing materials such as portland cement and plastics have reached a high stage of development. Failures of this type are probably due almost always to extraneous causes such as mud contamination rather than to faulty cementing material. Vertical coning can and obviously does occur. However, the usual occurrence of thin impermeable streaks in sand sections and the success with which open-hole drill-stem tests can be made near the gas-oil contact suggest that over-all effective vertical permeability, and in turn vertical coning, is less prevalent than frequently is assumed. Much has been written on failure by flowing out of the mud filter cake between cementing material and the formation. A filter cake is always present if, prior to cementing, mud has come in contact with a permeable formation at pressures exceeding the pressure head of the fluid it contains. Mechanical methods are in use for removing filter cake during the cementing operation? which undoubtedly are of

Jan 1, 1947

By R. H. Hiltz, R. W. Douglass

Large-grain specimens of iodide titanium prepared metal-lographically were stain etched using the technique of New York University as modified by Watertown Arsenal Laboratories. Orientations of grains showing an abnormal response to stain etching were determined by back-reflection X-ray techniques. X-ray results showed that a-titanium grains, oriented such that their basal planes were parallel to the polished surface, have a slower reactivity to stain etching than any other orientation. Grains oriented such that their basal planes made small angles with the polished surface exhibited reaction rates between that of the true basal orientation and the normal rate. As the angle with the surface increases the reactivity increases up to a maximum angle of 14 deg. Basal planes making an angle with the surface of greater than 14 deg show normal reactivity to stain etching. These data, plus work on polycrystalline specimens, indicate that the oxidation rate of titanium might be reduced by correct alignment of crystal planes. ThE earliest observed phenomenon in the micrography of titanium was the occurrence of a grains which exhibited no birefringency. Even though a titanium possesses a hexagonal-close-packed structure and should be optically anisotropic, it can appear optically isotropic, when the crystal is so oriented that its intersection with the polished surface is perpendicular to the axis of symmetry. During the develoment of color staining techniques for titanium: it was noted that the a phase did not stain uniformly. Staining of specimens of commercially pure titanium resulted in a micro-structure of blue-colored grains, among which were randomly oriented a few grains exhibiting colors between the initial yellow and the final blue color. Under polarized light, these off-colored grains appeared to be optically isotropic. More intense study with polarized light, however, showed only the yellow grains to be isotropic. The intermediate colored grains exhibited weak birefringency, which at first glance is not detectable due to the strong birefringency of the surrounding structure. Aminoff2 and Straumanis3 have previously shown that in zinc the basal orientation is less reactive than other orientations. Leidheiser4 showed the same thing to be true for the hexagonal-close -packed configuration of cobalt. Thus, it would appear that the basal-plane orientation is responsible for the abnormality in stained titanium. Later work by Leidheiser5 on cobalt has shown that other planes besides the basal plane exhibited reaction rates slower than the normal rate. Reported planes were the (100), the (1011) and several planes making small angles with the basal plane. The last observance appears not to be due to the reactivity of the reported plane but due to the reactivity of the basal plane which is very close to being parallel to the surface. There are, then, two possible explanations for the range of colors observed in stain-etched a titanium. Since extensive research on the effect of orientation on surface reaction has failed to provide any definite trend, these two explanations are not adequate in themselves. Planes showing the retarded reactivity differ not only for different crystal structures but for metals of the same crystal structure and even for different reactions of the same metal. Tragert,6 Leidheiser,7 Tammann,6 and wagner9 have shown copper to exhibit retarded reactivity on the (111) plane. However, Leidheiser10 has shown that under other conditions the retarded reactivity of copper is associated with the (100)

Jan 1, 1960

By M. S. Burton, G. V. Smith, A. Rosen

The kinetics of re crystallization and the effect of recovery on recrystallization of pure iron were investigated within the temperature range of 517" to 632 OC. Grain growth and activation energies were also studied. Two stages can be distinguished during recrystallization; the first is gvowth-controlled and the second is nucleation-controlled. The extent to which the first stage succeeds before the second stage begins depends on both temperature of recrystallization and temperature of recovery. The softening of cold-worked metals and alloys due to transformation of the deformed crystals to strain-free equiaxed grains during annealing is well-known, and early inestiators established that recrystallization kinetics is strongly influenced by minute quantities of impurities. Generally, it is believed that impurities decrease the rate of recrystallization and the rate of grain growth. To understand the basic phenomena of recrystallization, investigations should be on pure materials. Most of the research on high-purity materials has been on metals having the fee Bcc materials, and especially high-purity iron, have been studied only in recent years. It is known that recovery may influence recrystalliation;" however, no general description of the influence, applicable to all materials, has been presented. This paper presents results of a study of the recrystallization kinetics of high-purity iron, after 60 pct cold deformation by drawing, with particular reference to the influence of recovery on the rates of recrystallization and grain growth. From observations of these rates, conclusions are drawn concerning nucleation. MATERIAL AND EXPERIMENTAL PROCEDURE Preparation of Material. High-purity iron, prepared by zone refining of vacuum-melted electroiytic iron at Battelle Memorial Institute under sponsorship of the American Iron and Steel Institute, was used in this study. Table I gives the reported chemical analysis of the material, taken at a point near the last molten zone and thereby rep- resenting the maximum impurity level for the entire bar. Prismatic specimens, approximately 10 x 10 X 50 mm, were sawed from the 50-mm-diam bar, perpendicular to the zone-refining direction, and turned to cylindrical shape. These specimens were sealed in quartz capsules under vacuum, approximately 10"e mm Hg, austenitized at 930° C for 15 min, slowly cooled, removed from the capsules, and cold-worked in air by swaging to approximately 20-pct reduction of area. The encapsulating, austenitizing, and swaging operations were repeated two additional times, after which the samples were encapsulated, austenitized, and cold-drawn to 60-pct reduction of area. A further vacuum anneal at 630°C for 120 min and cold drawing to 60-pct reduction of area produced wire 2.8 mm in diameter. The drawn wire was electropolished to remove deformed material on the surface, after which it was sawed into 4-mm-long specimens for the recrystallization study. Microscopical examination before the final cold reduction revealed equiaxed grain structure with very fine grains in a thin layer near the surfaces of the specimen and nearly uniform ASTM 3-4 grain size in the center. Recrystallization Heat Treatment. a) Direct Recrystallization of Cold-Worked The 60 pct cold drawn iron specimens were recrystallized at five temperatures, 517, 556, 590°, 612, and 632C, in a lead bath covered with graphite (the temperature was controlled to 1°C). Specimens were treated for twelve different times at each temperature, and all were water-quenched after heat &eatment. b) Recrystallization Following Preliminary Recovery Heat Treatment. After cold working, specimens were sealed into quartz capsules under vacuum, 105 mm Hg, and recovery-annealed at 362", 400", and 440°C for 20 hr prior to recrystallization. No evidence of recrystallization was found

Jan 1, 1964

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.'-4 Samsonov et al.' reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami's Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965

Jan 1, 1969

By W. P. Saunders, W. R. Hibbard, G. H. Eichelman

Interest in the various products of the austenite eutectoid transformation in iron-carbon alloys, particularly as produced by the isothermal sub-critical techniques introduced by Davenport and Bain,' has resulted in the application of similar heat treatments to other eutectoid transformations. Studies o f the beta copper-aluminum alloy eutectoid transformation revealed microstructures very similar to those found in iron-carbon alloys. Investigations5t6 of the kappa phase in the copper-silicon alloy system have established the eutectoid type transformation of this phase into terminal alpha and intermediate gamma phases. This transformation has been reported5 as forming a eutectoid type structure in a very sluggish manner by a long time isothermal treatment. The purpose of the present investigation is to study the products of the kappa eutectoid transformation as affected by transformation temperatures by means of microscopic and hardness methods. Preparation of Alloys The copper-silicon alloy equilibrium diagram is shown in Fig 1. The kappa field converges to a minimum silicon solubility at the eutectoid composition and all other completely kappa alloys are hypereutec-toid. Thus, kappa decomposition involves first the proeutectoid precipitation of gamma, followed by the eutectoid transformation of a lower silicon content kappa (5.2 pct) Smith6 has indicated that alloys containing between 5.4 and 5.7 pct silicon could be hot rolled, but that the latter composition was desirable in order to permit a wider kappa temperature range. The alloy was prepared by adding Baker's commercially pure silicon to an ingot of copper-silicon alloy containing 2.34 pct silicon remaining from the investigation of Brick, Martin and Angier.' Following the casting techniques of Krynitsky, Saunders and Stern,s the ingot was melted under a heavy layer of dried charcoal in a clay-graphite crucible in a gas-fired pot furnace. Small lumps of silicon were held under thc melt surface with a graphite rod. After the silicon had dissolved, the alloy was chill-cast and then remelted without a cover, stirred thoroughly, skimmed and poured into a preheated cast iron mold. The cast microstructure is shown in Fig 2. The casting, 10 X 4 X K in., was annealed at 750°C for 21 hr and furnace cooled, About }{& in. was milled from all surfaces. The plate was cut in half longitudinally and the bottom half analyzed by A.S.T.M. and The composition by weight was as follows: copper 94.24 pct, silicon 5.56 pct, iron 0.11 pct.

Jan 1, 1949

By W. H. Yarroll

This paper presents a general discussion of the utility of the statistical technique known as multiple correlation, and gives three specific examples of its application. The first demonstrates the most simple form, or straight-line, multiple correlation. The other two demonstrate multiple correlation analysis in best-fitting third-degree parabolas. With the increasing availability of digital computers, the method becomes entirely feasible where heretofore its use was impractical. The advantages of the method are discussed, and curves are presented which were developed by computerizing the regression equations developed in the examples. The method described in this paper is for use with complex systems, and the examples given are complex metallurgical systems. This subject falls under the general classification of cybernetics, which is defined' as "the science of control and communication, in the animal and the machine." Machine, in this case, can include chemical and physical processes which take place within machines and processing equipment of all kinds. The classical approach to scientific investigation has been the construction of simple models and the changing of variables one at a time. This method is wholly inadequate for obtaining useful information from the complex systems of modern technology including many of our flotation and hydrometallurgical processes. Cybernetics offers the method by which complex systems which have been implemented as an art in the past can now be analyzed with all the discipline of a science. Mathematical techniques for achieving multiple correlation analysis have decided advantages over some of the other statistical methods.2-4 Multiple correlation does not require a series of experiments that have been rigidly planned as do many of the other statistical methods. For this reason, it can be used effectively for interpretation of information from op- erating plants, where planned experiments are impractical, as well as for laboratory experiments. First-degree multiple correlation has been used for many years, and was useful, but limited to linear or nearly linear relationships. The technique described in this paper provides a method for analyzing systems which may be non-linear. This particular technique is multiple correlation analysis in best-fitting third-degree parabolas. It is quite possible that lack of reference to the technique has been due to the overwhelming mass of computations it requires even for relatively simple problems. With the advent of computers, however, its use has become entirely feasible. For the benefit of those who may not be familiar with the subject, it might be well to pause at this point to discuss multiple correlation analysis — what it is and what it achieves. To go back to the old familiar fitting of a set of points with a best-fitting straight line by the least squares procedure, it is conceded that this a good method where there is only one independent variable influencing the dependent variable under consideration, and providing that the relationship is linear. In most fields of investigation, however, there are usually a number of factors exerting important influence, and they frequently bear relationships with the dependent variable other than straight line. Under these conditions, it is easy to see how misleading a simple correlation study might be. Multiple correlation can be used for any number of variables. Within the experience of the writer, this technique has been used to establish regression equations for determination of carbon rate, burden permeability, and production rate on iron blast furnaces, production rate on open hearth steel furnaces, life of molds for steel ingots, rolled steel tensile strength and various defects in rolled products, the performance of ore dressing equipment, and optimization of extractive metallurgical process variables. The discovery of mathematical correlation does not prove, per se, true cause-and-effect relationship, but simply establishes a hypothesis. If the regression equation can be used to make successful predictions of what will happen with future arrays of independent variables, then one can feel reasonably assured that true cause-and-effect relationships have been discovered.

Jan 1, 1968

By T. S. West

Completion and production data presented for three wells in the Oakville area of Live Oak County, Texas, which were completed near the gas-oil or water-oil contact, indicate that coning may not be as prevalent a cause of failure in such cases as is commonly assumed. Failure in the cases discussed is indicated to be due instead to: (I) erosion of the formation, (2) flowing out of mud filter cake, or (3) failure of the cement. An open-hole gravel-pack type of completion procedure is proposed for preventing failures of this kind by preventing movement of all solid material in the space in which completion is made. Various combinations of layers of gravel, sand, and cement are utilized for this purpose. Experimental results and theoretical discussion as to the applicability of gravel pack completion are included. Introduction This paper is primarily a study of the reasons for failure of oil-well completions near the gas-oil or oil-water contact, and suggests a procedure for increasing the efficiency of this type of completion. The value of improvement in completion effectiveness near the gas or water zone is not confined, however, to wells of relatively thin oil columns. Thick oil columns become thin as depletion progresses. It would seem to follow that the minimum distance from the gas or water zone at which completion can be made in a new well indicates the limit to which depletion may be carried in a well having an oil column of any initial magnitude. Only four ways can be postulated in which high gas-oil or water-oil ratio can initially occur if the zone exposed for production is within the oil column: 1. Failure of the cementing material. 2. Vertical coning. 3. Failure along the boundary between the cement and the wall of the well. 4. Failure of the formation comprising the wall of the well. Cementing materials such as portland cement and plastics have reached a high stage of development. Failures of this type are probably due almost always to extraneous causes such as mud contamination rather than to faulty cementing material. Vertical coning can and obviously does occur. However, the usual occurrence of thin impermeable streaks in sand sections and the success with which open-hole drill-stem tests can be made near the gas-oil contact suggest that over-all effective vertical permeability, and in turn vertical coning, is less prevalent than frequently is assumed. Much has been written on failure by flowing out of the mud filter cake between cementing material and the formation. A filter cake is always present if, prior to cementing, mud has come in contact with a permeable formation at pressures exceeding the pressure head of the fluid it contains. Mechanical methods are in use for removing filter cake during the cementing operation? which undoubtedly are of

Jan 1, 1947

By R. S. Kinasevich, D. D. Crabtree, D. W. Fuerstenau, T. P. Meloy, A. L. Mular

This paper presents details of the concept that size reduction in comminution machines takes place by three mechanisms; namely impact, abrasion, and chipping grinding. Experimental evidence is presented to show that each of these comminution mechanisms produces particles of a characteristic size distribution. The actual product from a comminution device has been postulated to be the result of a composite of these three types of mechanisms. Composite curves are demonstrated for a material following the Gaudin-Schuhmann, Gaudin-Meloy, and Rosin-Rammler size distributions. About forty years ago, Gaudin1 showed that grinding may be considered a combination of impact and attrition. Since that time, major efforts have been devoted to studies, both experimental and theoretical, of impact and compression fracture, while attrition has been almost wholly neglected, at least quantitatively. A significant attempt to distinguish between attrition and impact grinding is the work of Tanaka2 in Japan. By means of an instrumented abrasion grinder and a drop weight device, he determined coefficients relating the increase in surface area of various materials to the energy expended by the two methods of comminution. He showed that physical properties of a material determine its response to attrition and impact grinding. By extending his ideas to ball milling, he concluded that to a large extent the basic comminution process in a ball mill is due to the impact of falling media. Because Tanaka used a mass of particles in his drop weight device, however, he did not obtain pure impact size reduction. The purpose of this paper is to define basic mechanisms of size reduction, to verify that each has a characteristic and meaningful distribution curve, and to show how a combination of these mechanisms results in a size distribution very like that produced by grinding mills. DEFINITION OF COMMINUTION MECHANISMS The product from a grinding device will be considered to be the sum of the contributions resulting from the action of three basic mechanisms of size reduction which operate in a ball and rod mill. These are impact grinding and two forms of attrition, namely abrasion grinding and chipping grinding. Each is defined below. Impact Grinding: If a straight line is obtained when the cumulative weight fraction finer than a given size is plotted on log-log paper as a function of that size, the slope of the line is defined as the distribution modulus. A number of investigators 3,4,5 have shown that impact fracture of single specimens of different composition and shape results in a distribution of daughter particles that exhibit a distribution modulus of unity. This has also been true for materials broken in slow compression. Moreover, under slow compression or impact fracture conditions, theoretical distribution equations6*' which approximate the Gaudin-Schuhmann distribution when the distribution modulus is close to unity agree reasonably well with the experimentally obtained products. If one now considers a comminution process where many impact or compression fracture events are taking place, then any rational summation of the individual events yields, in the finer size range, a Gaudin-Schuhmann distribution whose distribution modulus is also unity. If the size distribution of the product from a mill has a distribution modulus of unity, it is implied that particles are fractured in a manner which results in a comminution event having a distribution like that obtained for the breakage of single specimens. These impact events would occur when a particle is smashed between balls or between a ball and the mill liner. Attrition, on the other hand, is that form of grinding which cannot be called impact grinding, and comprises both abrasion and chipping grinding. Abrasion Grinding: Abrasion is a form of surface wear resulting when particles rub against each other or against balls or the mill liner of a tumbling mill, somewhat like a piece of wood being rubbed over a piece of sandpaper. The surface wears at a more or

Jan 1, 1964

By A. L. Jr. Pozzi, A. O. Garder, D. W. Peaceman

A new numerical method is proposed for the solution of multidimensional miscible displacement problems. Besides the usual stationary grid associated with numerical procedures, the method uses moving points for which positions and concentrations are computed each time step. Based on the method of characteristics for treating combined transport and dispersion, the method applies equally well to any number of dimensions and, in contrast with other numerical procedures, properly takes into account the physical dispersion, no matter how small. Extensive tests show that accurate solutions of one-dimensional problems can be obtained over a wide range of values of the dispersion coefficient, including zero. They also show that the moving points do not need to be uniformly spaced, and that increasing the number of moving points beyond 2/grid interval does not significantly improve the accuracy of the solution. Two-dimmsional calculations using the new method were carried out to simulate laboratory model displacements in which gravity caused overriding of solvent. Good agreement between observed and computed profiles and measured and computed concentrations of produced fluid was obtained for a viscosity ratio of 1.89; at higher viscosity ratios, fair agreement was obtained Computed results were found to be significantly affected by vertical dispersion, and negligibly affected by dispersion in the direction of flow, in agreement with conclusions based on experimental observations. INTRODUCTION Although miscible displacement processes are potentially of great economic significance, limited progress has been made in developing mathematical methods for predicting the outcome of a solvent flood. Because of the complexity of the partial differential equations which describe multidimensional miscible displacement, numerical methods are a natural approach to their solution. The task of finding suitable numerical approximations to one of the partial differential equations, which involves both dispersion and convective transport, has been particularly difficult. Dispersion in the absence of transport is described by the heat flow equation, a second-order equation of parabolic type. This equation has been very successfully treated by numerical methods. Transport in the absence of dispersion is described by a first-order equation of hyperbolic type. This equation has been treated numerically with some success in one dimension, both by Lagrangian and Eulerian techniques, 1.2 but extension to two or more dimensions has not been satisfactorily accomplished. Usually one of two things happens: either the numerical solution develops oscillations or it becomes smeared by artificial dispersion resulting from the numerical process. When transport and dispersion are considered simultaneously, this numerical dispersion may dominate the low physical dispersivicy that generally characterizes miscible displacement. Stone and Brian2 have developed a new difference equation for treating combined transport and dispersion in one dimension. By suitable choice of certain parameters, they succeeded in markedly reducing both oscillation and numerical dispersion. However, a satisfactory extension to higher dimensions has not yet been found. Peaceman and Rachford3 presented a centered-in-time and centered-in-distance difference equation combined with a 1,transfer of overshoot" procedure which was demonstrated to work well in one dimension. The technique was applied to the two-dimensional miscible displacement problem, but subsequent calculations with zero dispersivity showed little change in results compared with the calculations they presented. This indicates that their method involved a numerical dispersion of the same order as the physical dispersion. The present paper describes an alternate method for solving the combined transport-dispersion

Jan 1, 1965

By Charles A. Ashburner

The Bradford Oil District lies in the northern part of McKean County, Pa., and the southern part of Cattaraugus County, N. Y. Although petroleum was first found in the producing sand in 1871, it was not until the early part of the year 1875 that a productive horizon was acknowledged to exist, even by those most largely interested in the production of the crude oil. It has been reported to me that the first well drilled in the valley of the Tuneangewant Creek (commonly called Tuna Creek) was drilled by F. E. Dean and brothers in 1865. This well was located on the Shepherd farm, near the present site of Custer City. One hundred and sixty feet of drive pipe was used, and the hole was drilled to the depth of 900 feet. The producing sand at Custer City is found about 1130 feet below the level of the railroad track. The Shepherd farm well was therefore abandoned over 200 feet above the top of the oil sand. The next well was drilled by the Dean brothers on the Clark farm at Tarport. Drilling was stopped at a depth of 605 feet, or over 400 feet above the top of the oil sand. In the year 1862 the old Bradford well, since known as the Barnsdall well, was drilled to a depth of 200 feet with a spring pole, and then abandoned. In the spring of 1866 the citizens of the village of Bradford concluded to club together and sink the Barnsdall well deeper. It was drilled to a total depth of 875 feet, or to within 150 feet of the Bradford producing sand. All of these wells were drilled with the expectation of finding the Venango County oil, and at

Jan 1, 1879

By Chas. A. Ashburner

THE Bradford Oil District lies in the northern part of McKean County, Pa., and the southern part of Cattaraugus County, N. Y. Although petroleum was first found in the producing sand in 1871, it was not until the early part of the year 1875 that a productive horizon was acknowledged to exist, even by those most largely interested in the production of the crude oil. It has been reported to me that the first well drilled in the valley of the Tuneangewant Creek (commonly called Tuna Creek) was drilled by F. E. Dean and brothers in 1865. This well was located on the Shepherd farm, near the present site of Custer City. One hundred and sixty feet of drive pipe was used, and the hole was drilled to the depth of 900 feet. The producing sand at Custer City is found about 1130 feet below the level of the railroad track. The Shepherd farm well was therefore abandoned over 200 feet above the top of the oil sand. The next well was drilled by the Dean brothers on the Clark farm at Tarport. Drilling was stopped at a depth of 605 feet, or over 400 feet above the top of the oil sand. In the year 1862 the old Bradford well, since known as the Barnsdall well, was drilled to a depth of 200 feet with a spring pole, and then abandoned. In the spring of 1866 the citizens of the village of Bradford concluded to club together and sink the Barnsdall well deeper. It was drilled to a total depth of 875 feet, or to within 150 feet of the Bradford producing sand. All of these wells were drilled with the expectation of finding the Venango County oil, and at

Jan 1, 1879

By C. O. Babcock

In this Bureau of Mines report, the authors present the results of laboratory tests on the burst proneness of coal. Many researchers have studied the violent breaking of large coal masses in underground mines, called bursts, but the causes remain uncertain. They have often assigned to geology and gas pressure the causative roles. The objective of this work is to show that stress can produce bursts in many coals if constraint is necessary for pillar survival and is suddenly lost. We tested coal samples from 15 mines, in 11 coal seams, in six states in the laboratory, and 13 were made to burst. These bursts were produced in several ways, but segmented steel platens were used in the tests reported. Two parameters analogous to the momentum and kinetic energy were used to rank the burst proneness of the coals tested. Tangential strains over the lower surface of the model coal pillar were measured to reveal a periodic slipping prior to the burst. High-speed motion pictures (350 frames per second) reveal the burst behavior in slow motion. We propose a modified Mohr-Coulomb stress-failure criterion to describe the burst behavior. When the horizontal constraint is suddenly lost with little change in the vertical stress, the Mohr stress circle increases in size dynamically, exceeding the static failure condition. When the inertia of the coal mass is overcome, a burst occurs. We conclude that most coals can be made to burst and that such bursts can be expected in mining at increasing depths.

Jan 1, 1984

By George A. Moore

A recent survey of existing analytical results, and an attempt to correlate them with each other and with the known history and behavior of the samples, indicated that none of the commonly applied methods could be considered established as intrinsically reliable. It was. therefore, desired to attempt to establish the reliahility of some one method by external evidence. If this were to be accomplished, other methods could then be evaluated in terms of the method establibhed. The correct method was accordingly to be chosen without regard for cost, speed, or convenience; with the requirements for routine application to be reserved for 1ater consideration. The method of total combustion was chosen and submitted to a limited number of tests against primary standard samples. Considerable experimental difficulty was encountered, indicating that additional work on the experimental arrangements is desirable. While the work to (late by no means represents a completed investigation, it is helieved that the combustion method is basically sound and that its development should be continued. Choice of Method Of the several available methods, mechanical disintegration. electrochemical methods'2'3 modifications of the Sieverts experiment,% and vacuum fusion, were all judged to contain one or more factors of un- certainty not at present completely cvaluated or suhject to complete control. These methods, therefore, were considered currently unsuitable for referee purposes. Solid evolution was considered to be of doubtful significance when conducted in the alpha range. A reasonable chance for a true analysis was found for evolution in the gamma range. Preliminary tests have indicated a very slow rate for evolutioll from gamma iron. indicating a running time of possibly 100 hr. for a one-centimeter sample. Difliculty in distinguishing such slow. evolution from blank gas was anticipated, hence the method was not consitlerctl the most suitable for the present purpose. The combustion method was evaluated as being most sound on fundamental principles. The only important unknown would be to determine that the iron oxide formed did not occlude water at the tcmperaturv of the combustion.with the odvious precautions of using a sound and clean specimen, providing a system sufficiently tight to give acceptable blanks in longtime runs, and providing a suficicntly sensitive measuring system, reasonable, precise, and truthful analytical results could be logically expected. Apparatus The equipment as originally operated is shown in Fig. I, and the glassw-are in its latest modification in Fig. 2. The sulphuric acid drier and small safety tube in the upper right of Fig. I were replaced by a KOH drier and combined manometer safety tube, to permit operation at reduced

Jan 1, 1945

By Maurice E. Peloubet

This discussion of accounting will describe the statements and the information that the accounting system produces, from the point of view of those who use such systems rather than of those who prepare them and who do the detail and technical accounting work. In any well organized mine, quarry, or other enterprise exploiting a mineral deposit, no matter how small, some clerical and accounting work must be done. Miners and other employes must be paid, supplies must be purchased and issued, and various tax and information returns, which even the smallest enterprise must file, have to be prepared. In this chapter it is assumed that the enterprise has employes of this type and that they understand the fundamentals of record keeping and accounting. It would be impossible here to give sufficiently full explanations to enable a man with no previous clerical and accounting training to set up and operate an accounting and cost system for even the simplest extractive operation. Rather, we shall hope first, to tell the investor and the operator, from the chief engineer or president down to a subforeman, what to expect from the accounting statements and records and how to use this information in his daily work; and second, that it will enable the man with some knowledge of accounting or bookkeeping, but with little or no experience in any extractive industry, to set up and operate a satisfactory system for a mine or other extractive enterprise. For readers who wish to go further, the bibliography at the end of this chapter contains many references. The emphasis has, therefore, been placed on the statements to be produced and the purposes for which they are to be used rather than the underlying books and records. These are, with a few exceptions which will be described later, essentially what might be found in any industrial enterprise and would probably, in the extremely small enterprise, consist of handwritten journals, ledgers, analysis books, payroll books, and stores ledgers. In the larger enterprise, various types of mechanical accounting would be introduced in proportion to the complexity of the operation.

Jan 1, 1959

By S. S. Clarke

THE sheet-ground deposits of the TriState district, because they are fairly uniform in thickness (7 to 11 ft.)-rather flat, with an easy dip to the west-and cover a large acreage, offered a problem of improved transportation. Heading advance in this kind of mine is very rapid and track haulage requires a larger crew of trackmen than do other mines, and a heavy investment in track. The use of some type of rubber-tired truck equipment for underground haulage was under consideration for some time by the Eagle-Picher Mining and Smelting Co. The nature of some ore bodies made them not adaptable to truck haulage and some mines that did offer possibilities were equipped with other types of haulage, and the expected savings by the use of trucks did not offset the loss of investment that would be incurred in discarding other equipment. The decision was made to sink a new shaft, designed for skip hoisting, on the Blue Goose ore body, and then develop truck equipment. DEVELOPING TRACTORS AND TRAILERS A study was made of internal-combustion engines for power units in the tractors, but the extreme difficulty of controlling air circulation, and the heavy cost of drilling large churn drill holes for blower installations, led to the adoption of a tractor with a storage battery. The storage-battery tractor that was on the market for mine haulage was impossible to obtain because all were needed for defense work. Several standard electric-truck chassis were purchased and rebuilt in the Eagle-Picher shops. The steering wheel was shortened and set vertical, permitting the driver's seat to be moved forward, and the frame was shortened enough to take the battery box and the fifth wheel support that carried the gooseneck of the dump trailer. The fifth wheel, or turntable, is of the ball and socket type. Fig. I shows the ball fastened to the gooseneck. The socket is split to permit introduction of the ball and is held by through-bolts, and the socket is welded to a ½ -in. plate, which in turn is attached to the tractor frame. Smaller wheels and tires were put on to reduce over-all height. If it had been necessary, the springs could have been reversed, or taken off entirely, to gain additional clearance. The tractors are equipped with 48-cell, 23-plate, 400-A.H. batteries. With the initial tonnage and mileage, the batteries were about 50 per cent down at the end of a shift. Tractors have truck tires 7.50 by 20, 8-ply, front and rear, the rear being dual. After four months of use, the tires are beginning to show signs of failure.* In

Jan 1, 1942

By J. B. Newkirk, A. H. Geisler

Certain of the permanent magnet alloys provide ideal systems for the study of the kinetics of the precipitation reaction and the correlation of structure with properties. One such system, Cu-Ni-Fe, was found by Bradley1,2 to exhibit a coherent transition state in the precipitation process analogous to that reported for Al-Cu alloys somewhat earlier.3 The attractiveness of some perrnanent magnet alloys for study lies in the fact that vertical sections of the ternary phase diagram in certain regions of composition (Fig I) have as their prototype the binary Ni-Au diagram. Alloys of this type decompose into products that have the same crystal lattice type but only slightly different lattice parameters. The advantages that such alloy systems oA&apos;er for study over the usual in which an intermetallic compound is formed are many: 1. Since the precipitate has the same crystal strutture as the matrix, complex atomic movements are not required to form the new lattice. 2. Similarly, complex orientation relationships are not involved for both the matrix and the precipitate would be ex. petted to have the same orientation. 3, Small &,registry of the decomposition products at equilibrium (in contrast with Cu-Ag alloys) is conducive to extensive coherent growth in the transient state and thus the transition lattice can be detected by the usual X ray diffraction methods. 4. Finally, the relative quantities of precipitate and depleted matrix can be varied from 0 to 100 pet* thus permitting wide freedom for the study of the effect of cornposition on coherent growth and properties. In the Cu-Ni-Fe alloys of appropriate composition, the face-centered cubic precipitate and also the depleted matrix when first formed are coherent with the parent matrix.1&apos;2 The two have the same <Jo parameter as the original matrix but they are both tetragonal; the precipitate has an axial ratio c/a < I while that of the depleted matrix is c/a > I. When coherency is lost they assume the normal face-centered cubic structure with the depleted matrix having a lattice parameter greater than the original matrix and that of the precipitate less. Such a mechanism would also be expected for CU-Ni-CO alloys because of the similarity in constitution but this had not been demonstrated. The Present investigation was conducted on a CU-Ni-CO alloy. The constitution diagram and magnetic properties of these alloys have been fairly well established, however, no previous determinations of mechanism of precipitation and no correlation of structure with properties had been made. Thus, an alloy of this system Was chosen for a comprehensive investiga-

Jan 1, 1949