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By Christopher W. Schram, Allan B. Tanner, Frank E. Senftle, George R. Boynton, Philip W. Philbin

A borehole sonde using a 252Cf neutron source and a Ge(Li) gamma-ray detector was field tested in a coal bed in Belmont County, Ohio, to ascertain whether such a device could be useful as a coal-exploration tool. As the sonde was lowered into the borehole, successive spectra were accumulated over short time intervals. The intensities of the capture gamma rays from hydrogen and of decay gamma rays from aluminum were determined simultaneously in each spectrum. A log of the intensities versus depth shows the depth and thickness of the coal bed. With the sonde stationary at points above, in, and below the coal bed, capture gamma rays were measured to show the variation in concentration of certain elements. From the spectrum recorded in the bed, a complete ultimate analysis, the percent ash content, and the heat content were determined without recourse to an external standard. Delayed gamma-ray analyses of the core were also made on the surface in the vicinity of the borehole in a fixed-geometry irradiation facility wing the detector in the borehole sonde. The concentrations of 10 elements were determined by this method on a coal split from the drill core. These experiments show that it is feasible to use a 252Cf- Ge(Li) borehole sonde as an aid in coal exploration.

Jan 1, 1979

By C. R. Austin

IN a recent paper1 the authors presented information on a refinement of the Rohn type of creep test with data on pure iron that exemplified the behavior of the apparatus. The present paper extends that work to nickel and cobalt and to the examination of the comparative high-temperature properties of two widely used commercial alloys. Careful attention has been given to the effect of plastic deformation in decreas-ing creep rate, using the elementary metals iron, nickel and cobalt for purposes of analysis. In any, endeavor to develop new materials for high-temperature service one soon encounters a real problem as to the sort of test to be employed in evaluating the commercial possibilities of the alloys. At one time it was considered satisfactory to determine the tensile strengths at elevated temperatures and to use these values as a criterion for the commercial application of the alloys. More recently the proportional limit has been used as a means of classification. Data obtained from a form of bend test has also shown promise as providing a "merit index" of high-temperature serviceability.2 Koerber and Pomp3 state that since the influence of testing time is small, the high-temperature yield point of steel furnishes sufficiently reliable and concordant values up to about 350° C. (and a maximum of

Jan 1, 1934

The most extensive oil shale development program ever undertaken in the United States has been that carried out by Colony Development Operation at Para- chute Creek in western Colorado. Field development goals were completed this spring, with the remainder of the $24 million joint venture program, primarily engineering, environmental and economic analysis, due to be finished by the end of 1972. Upon completion of the overall program, a decision concerning a commercial venture is expected. This program points up the increasing attention being focused on oil shale as a source of crude oil and energy for the U.S. at a time when the nation's supply of oil produced by conventional methods is far from adequate to meet the demand. The oil shale reserves of the Green River formation in Colorado, Utah and Wyoming are the largest hydrocarbon reservoir. The Piceance basin of Colorado, alone, contains some 80 billion bbl of shale oil recoverable by modern methods in reserves more than 30 ft thick and containing at least 30 gal of oil per ton. The U.S. Geological Survey has estimated that the total shale oil reserves of the Green River formation in the states of Colorado, Utah and Wyoming is more than 600 billion bbl of oil in deposits containing at least 25 gal per ton of shale oil.

Jan 10, 1972

By Ernest Klepetko

A notable amount of fossil resin exists in many of the bituminous coal beds of Utah. The upper part of these show a marked concentration of resin, which occurs primarily in the fracture seams. In general, these seams are less than 1/8 in. thick, but it is not uncommon to find coal with areas as thick as 3/8 inches. The resin is of the hard kauri variety, with coloration varying from deep blood red to lemon yellow and almost colorless. There is also an almost black variety, which is not readily soluble in the same solvents as the lighter colored resins. These resins are valuable for many industrial purposes. When refined, they are suitable for uses similar to those for which lac resins are usually employed. They are particularly desirable for preparing dielectric varnishes. They are also desirable in preparing printing inks, waterproofing agents, special synthetic rubbers and rubber cements. They are especially suitable as an admixture in synthetic rubbers and cements, as they supply the essential tackiness the synthetics lack. The following chemical trade characteristics have been found by Inter-Chemical Co. research chemists in the refined resins: Specific gravity (melted)....... I .03 -I.06 Acid number.................. 6-8 Softening point, mercury method 160º-165ºC Iodine value (Wijs)............ 140-150 Refractive index............... 1.544 Color (Hellige, 25 pct toluol)... 14 Molecular weight, average...... 732 Purity, 99 + pct pure hydrocarbon "Unaffected by alkalies and resistant to one hour fusion with solid potassium hydroxide. Completely soluble in aliphatic and aromatic hydrocarbons. Insoluble in alcohols, ethyl acetate and other commonly used alcohols and esters. Compatible with natural and synthetic rubbers, chlorinated and cyclized rubbers, waxes, vegetable oils, mineral oils, rosin, ester gum, phenolic and modified phenolic resins and other natural and synthetic resins of like solvent solubility."* The recovery and refining of these fossil resins has been the subject of much research work and has intrigued many investigators. Broadly speaking, the problem involves separation of the resin from the coal into a very high-grade concentrate, and subsequent treatment of this concentrate to produce an acceptable refined resin for its various usages. Obviously it is also desirable to recover the residual coal without excessive size degradation. The late W. D. Green, concentration ennineeru for Combined Metals Reduction CO., obtained U, S. Patent No. 1773997 for the recovery of resin from coal through

Jan 1, 1948

By R. H. Olds, B. H. Sage

The formation volume and volume of the liquid phase of oil and gas obtained from four fields in the San Joaquin Valley have been investigated at pressures, temperature, and gas-oil ratios comparable to those encountered in underground reservoirs. All the fields covered in this investigation yielded a product of a gas-oil ratio in excess of 5000 cu ft per barrel and the gravity of the tank oil for the four fields in question varied between 52° and 63' API. The results of the investigation, together with analytical data concerning the composition of the oil and gas, are submitted in tabular form. Rough correlations of the formation volume as a function of pressure, temperature, and gas-oil ratio and of the retrograde dew-point pressure as a function of gas-oil ratio, temperature, and gravity of tank oil are presented. It was not found feasible to correlate simply the formation volume of the liquid phase as a function of the applicable variable. It is desired to emphasize that these correlations are considered applicable only to the range of conditions covered in this investigation and for systems of similar nature and composition. Introduction Information concerning the physical properties of mixtures of oil and gas from particular fields have often been employed in predicting the situations obtaining in underground reservoirs. One of the earlier studies of this nature was the work of Beecher and Parkhurst,1 while a more recent study of the Dominguez Field2 presented detailed volumetric data in the two-phase as well as in the single-phase regions. Although these studies were confined to individual fields, their results proved of value in application to other fields. It has recently been shown 3,4 that it is possible in the region of low gas-oil ratios* to correlate the volumetric behavior of naturally occurring hydrocarbon mixtures from a single geographical area with sufficient accuracy to be of industrial value. For this reason it is considered of interest to submit information concerning the volumetric behavior of oil and gas mixtures from four different fields in the San Joaquin Valley and, in combination with similar published data5 concerning mixtures of oil and gas from the Paloma field in the same area, to show rough correlations between the composition and the behavior of materials from these fields. This effort seems particularly worth while since all of the

Jan 1, 1947

By R. H. Olds, B. H. Sage

The formation volume and volume of the liquid phase of oil and gas obtained from four fields in the San Joaquin Valley have been investigated at pressures, temperature, and gas-oil ratios comparable to those encountered in underground reservoirs. All the fields covered in this investigation yielded a product of a gas-oil ratio in excess of 5000 cu ft per barrel and the gravity of the tank oil for the four fields in question varied between 52° and 63' API. The results of the investigation, together with analytical data concerning the composition of the oil and gas, are submitted in tabular form. Rough correlations of the formation volume as a function of pressure, temperature, and gas-oil ratio and of the retrograde dew-point pressure as a function of gas-oil ratio, temperature, and gravity of tank oil are presented. It was not found feasible to correlate simply the formation volume of the liquid phase as a function of the applicable variable. It is desired to emphasize that these correlations are considered applicable only to the range of conditions covered in this investigation and for systems of similar nature and composition. Introduction Information concerning the physical properties of mixtures of oil and gas from particular fields have often been employed in predicting the situations obtaining in underground reservoirs. One of the earlier studies of this nature was the work of Beecher and Parkhurst,1 while a more recent study of the Dominguez Field2 presented detailed volumetric data in the two-phase as well as in the single-phase regions. Although these studies were confined to individual fields, their results proved of value in application to other fields. It has recently been shown 3,4 that it is possible in the region of low gas-oil ratios* to correlate the volumetric behavior of naturally occurring hydrocarbon mixtures from a single geographical area with sufficient accuracy to be of industrial value. For this reason it is considered of interest to submit information concerning the volumetric behavior of oil and gas mixtures from four different fields in the San Joaquin Valley and, in combination with similar published data5 concerning mixtures of oil and gas from the Paloma field in the same area, to show rough correlations between the composition and the behavior of materials from these fields. This effort seems particularly worth while since all of the

Jan 1, 1947

By J. E. Elliott, K. O. Miller

Solubility studies were carried out to establish the phase distributions for various Fe-Ni-Pb-C alloys at temperatures where the metallic components exist as liquid solutions. Temperature us composition diagrams for the Ni-Pb, Fe-Pb, Fe-Ni-Pb, and Ni-Pb-C systems are derived by employing various approximations in conjunction with the data. Results are summarized for 1550°C in a quaternary phase diagram of the Fe-Ni-Pb-C system. BECAUSE surprisingly little information has been published on the phase diagrams of the Ni-Pb, Fe-Pb, Fe-Pb-Ni, and Fe-Ni-Pb-C systems, a study of these systems was undertaken to ascertain the important phase relationships in the temperature range of 1300" to 1550°C. Measurements were also made on the carbon-saturated systems in the hope that they would assist in the interpretation of the systems without carbon. This paper reports the results obtained from the simple equilibration of the various liquid and solid phases. EXPERIMENTAL PROCEDURE The experimental technique involved holding appropriati quantities of the metals in an alumina crucible, or in a graphite crucible when saturation of the melt with carbon was desired, for sufficient time at the desired temperature to ensure equilibrium. Then a sample of each liquid phase presen was drawn into a small-bore silica tube. This sample was withdrawn quickly from the furnace, cooled, and sent to the chemical laboratory for analysis. The cell assembly used is shown in Fig. 1. Durin the work on the Fe-Pb-Ni system, it was placed in a furnace wound with 20 pct Rh-80 pct Pt wire. This furnace eventually failed and subsequent studies were carried out between 1350" and 1475°C in a tube furnace heated by silicon-carbide resistance elements. A protective atmosphere of argon with approximately 10 pct hydrogen was supplied to the cell assembly at a gage pressure of 1 in. of water. Hydrogen was passed over palladized alumina and then anhydrous calcium chloride for purification. Argon was purified of oxygen and water vapor by passing it over copper gauze at 550°C and then through a calcium chloride drying column. The gases were mixed and redried before they entered the equilibration cell. Temperature was measured by calibrated Pt/Pt-10 pct Rh thermocouples and a Rubicon Type B potentiometer. The thermocouples were standardized against the melting points of pure nickel

Jan 1, 1961

By Ernest Klepetko

A notable amount of fossil resin exists in many of the bituminous coal beds of Utah. The upper part of these show a marked concentration of resin, which occurs primarily in the fracture seams. In general, these seams are less than 1/8 in. thick, but it is not uncommon to find coal with areas as thick as 3/8 inches. The resin is of the hard kauri variety, with coloration varying from deep blood red to lemon yellow and almost colorless. There is also an almost black variety, which is not readily soluble in the same solvents as the lighter colored resins. These resins are valuable for many industrial purposes. When refined, they are suitable for uses similar to those for which lac resins are usually employed. They are particularly desirable for preparing dielectric varnishes. They are also desirable in preparing printing inks, waterproofing agents, special synthetic rubbers and rubber cements. They are especially suitable as an admixture in synthetic rubbers and cements, as they supply the essential tackiness the synthetics lack. The following chemical trade characteristics have been found by Inter-Chemical Co. research chemists in the refined resins: Specific gravity (melted)....... I .03 -I.06 Acid number.................. 6-8 Softening point, mercury method 160º-165ºC Iodine value (Wijs)............ 140-150 Refractive index............... 1.544 Color (Hellige, 25 pct toluol)... 14 Molecular weight, average...... 732 Purity, 99 + pct pure hydrocarbon "Unaffected by alkalies and resistant to one hour fusion with solid potassium hydroxide. Completely soluble in aliphatic and aromatic hydrocarbons. Insoluble in alcohols, ethyl acetate and other commonly used alcohols and esters. Compatible with natural and synthetic rubbers, chlorinated and cyclized rubbers, waxes, vegetable oils, mineral oils, rosin, ester gum, phenolic and modified phenolic resins and other natural and synthetic resins of like solvent solubility."* The recovery and refining of these fossil resins has been the subject of much research work and has intrigued many investigators. Broadly speaking, the problem involves separation of the resin from the coal into a very high-grade concentrate, and subsequent treatment of this concentrate to produce an acceptable refined resin for its various usages. Obviously it is also desirable to recover the residual coal without excessive size degradation. The late W. D. Green, concentration ennineeru for Combined Metals Reduction CO., obtained U, S. Patent No. 1773997 for the recovery of resin from coal through

Jan 1, 1948

By C. V. Corless

WE are living at a period of the world's history in which social phenomena are on so vast a scale, are of so profoundly soul-searching a nature, and are occurring in such rapid succession in the great world drama in which we are both actors and spectators, that, in our efforts to obtain a rational point of view in relation to them, our minds may fail to discern the simple in the complex and our understanding is liable to be-come confused or even overwhelmed. To the social student whose scientific training has convinced him of the truth of the evolutionary law, Natura non facit saltum, it is neither the vast scale of the events; their deeply soul-stirring nature, nor their rapid succession that matters so much, as the discovery of the underlying principle or law in accordance with which the disintegration and reintegration, which are the two aspects of social evolution, or indeed of evolution everywhere, are occurring. He is most deeply concerned in seeking an answer to the question: Have we in the present great and perplexing upheavals in human society, whether regarded in Central Europe, in Russia, in Great Britain, or in America, a really new cause at work, or, have we, though on a very- large scale, merely new manifestations of the working out of an old principle? When we think of the appalling struggle in Europe, into which the world's greatest exemplar of democracy was finally drawn, no one has any hesitation in admitting that the great conflict was fundamentally a life-and-death struggle for self-preservation and self-propagation on the part of autocracy. The variations we meet with in the statement of the cause of the war arise mainly from differing distances of perspective: but in the last analysis all agree that the autocratic system of political government, which found its very soul and center in Prussian despotism, was consciously arrayed in a final "world-power-or-downfall" struggle against a love of freedom which was steadily widening and-deepening throughout the world, and particularly throughout those parts of the world where this love of freedom and justice has found expression in democratic institutions. It is not irrelevant to our discussion to recall in passing that this most imposing structure ever conceived by the human mind as an instrument of tyranny is lying today an irretrievable mass of ruins, completely over-

Jan 4, 1919

By W. M. Pierce

THE present work has been done in an endeavor to correlate and complete the data on the constitution of alloys of zinc with other common, metals, dealing exclusively, however, with the zinc-rich alloys in which the zinc content is between 90 and 100 per cent. This investigation has included the systems lead-zinc, cadmium-zinc, iron-zinc, copper-zinc, aluminum-zinc, nickel-zinc, manganese-zinc, cobalt-zinc, tin-zinc, and magnesium-zinc. The important ternary system zinc-lead-cadmium and the zinc corners of other ternary systems have been investigated in connection with this work but will not be dealt with here. Zinc does not form a single homogenous zinc-rich solid solution over any considerable range of concentration with any of the metals mentioned. A limited range of solid solubility is said,; by previous investigators, to occur in several cases and certain effects on the properties of zinc are attributed (with varying degrees of consistency among different writers) to the presence of certain other metals dissolved in zinc. The increasing use of rolled zinc and the possibilities offered by zinc as a casting alloy in certain fields have it made essential to determine precisely these equilibrium relationships. In carrying out this .investigation reliance was placed chiefly on two methods, conductivity measurements and microscopic analysis. The first method proved valuable in determining the existence and extent of solid solubility. The second method stands alone as a means of determining structural characteristics and supplements the first method in the measurement of solid solubility. The scleroscopic hardness of all conductivity specimens was measured partly for its value from the point of view of mechanical properties and partly; as a check on the conductivity curves in indicating the limits of solid solubility. No hardness curves are included in this paper, for in no case were they important in arriving at the constitution of any system.

Jan 2, 1922

By N. J. Themelis, P. Spira

The efficiency of the reverberatory furnace operation in producing. slags of 1020 copper content depends on the mixing and flow conditions in the bath. Radioactize-tmcer tests have indicated the jkaction of bath volume engaged inflow and the mixing conditions in the bath. The factors controlling the flow pattern of slag have been classified as laminar transfer flow, natrsral convection, and flou, due to the rapid addition or removal of slag.. Similarity criteria for model studies have been developed. The pyrometallurgical processing of copper begins with the smelting of either flotation concentrates, or direct-smelting ores which have been partially roasted to calcines. These materials are generally smelted in a reverberatory furnace, Fig. 1, and separate into two liquid phases, a sulfide matte and an iron silicate slag. he matte is tapped and subsequently reduced to metallic copper in a converter, while the reverberatory slag is usually discarded without any further treatment. Molten slag from the converting operation is returned intermittently to the reverberatory in order to recover its high copper content (1 to 3 pct Cu). The reverberatory furnace is about 115 ft long by 30 ft wide. In general, the solid charge is fed at intervals through openings along the sides of the roof and forms sloping banks from which the molten materials trickle down into the bath; the charge banks extend over a length of about 70 ft from the firing wall. The depth of the slag and matte layers varies from smelter to smelter; in the Noranda furnaces, the slag depth is 24 to 30 in., while the depth of matte at the taphole is about 20 in. Apart from smelting, the functions of the reverberatory are to recover most of the copper content in the converter slag by physical and chemical interaction with the furnace bath, and to provide adequate time for optimum separation between matte and slag. The efficiency of these operations depends on the mixing and flow conditions in the bath and is reflected on the copper losses in the slag. In the present study, the reverberatory furnace is considered as an open-channel chemical reactor and the driving forces for material transport through the bath are examined by means of flow and mathematical models. FLOW CONDITIONS IN THE REVERBERATORY FURNACE To facilitate the study of mixing conditions in continuous-flow reactors, two idealized patterns of flow have been accepted by workers in this field.' The term "backmix" flow is used to describe complete and instantaneous mixing in the reactor (perfect mixing); all particles have the same chance of leaving the system, independently of their time of entrance, and the fluid is uniform in composition throughout the vessel. On the other hand, "plug" flow, or "piston" flow, assumes that a fluid element moves through the reactor without overtaking or mixing with fluid entering at an earlier or later time. In addition to the two idealized patterns of flow, "deadwater" flow accounts for that portion of the fluid which is moving so slowly that it may be assumed to be stagnant. According to the definition by evensppiel,' the cut-off point between active and stagnant fluid may be taken as material which stays in the vessel for a period twice the mean residence time. The flow patterns in real vessels may be approximated by a combination of the above flows. Thus, the vessel is assumed to consist of interconnected flow regions with various modes of flow existing between them. The flow pattern may be determined directly from the flow paths of fluid through the essel. -However, the difficulty of obtaining and interpreting such information has led to the alternate approach of determining the residence time distribution of fluid elements by means of stimulus-response studies. The stimulus is provided by introducing a tracer in the inlet stream and the response by the record of the change in tracer concentration in the exit stream from the reactor. Such tests have been conducted in glass tank furnaces using either chemical7"9 or radioactive tracers1'-'' and, in one case, experiments have been reported for a metallurgical furnace.'"

Jan 1, 1967

By H. U. Schutt, J. M. Toguri

REGARDLESS of the degree of purification effected during the electrorefining of copper, a danger of re-introducing impurities exists in the operation of melting and casting of the refined copper. Logically only a combination of the purification and casting operation would remedy the situation. A well-known method of metal purification is the "Gross"-type process, whereby a volatile halide is produced, purified, and decomposed.' In the present case, this concept was used to remove the impurities rather than to form possible volatile copper halides. The object was to produce volatile halides of the impurities present and distill these away, leaving high-purity copper. It is interesting to note that such techniques are used in spectrographic procedures in order to shorten exposure time and enhance the density of impurity lines.' In the present investigation, copper hydroxy fluoride was used, since the temperature of decomposition of copper hydroxy fluoride and the melting point of copper nearly coincide. The fluorine released by the thermal decomposition of copper hydroxy fluoride purges the molten copper. Copper hydroxy fluoride was prepared by dissolving high-purity copper in nitric acid and adding hydrofluoric acid and ammonium hydroxide in the required proportions. The melt was made in a high-purity graphite crucible heated by an induction furnace. Trial experiments showed that impurities can be introduced from the crucible material. Therefore, preceding each cast, the crucible itself was cleaned by decomposing copper hydroxy fluoride and discarding the residual copper. Best experimental conditions were obtained by adding 30 g of copper hydroxy fluoride to 500 g of nor-

Jan 1, 1967

By Augustus Locke, Edward H. Perry

In the exploration of a copper deposit by drilling, obvious advantages are to be gained from a distinction between primary and secondary ore.' Perhaps the chief of these is the aid which such a distinction renders in determining where a given hole should stop. The copper assay, often a sufficient guide, cannot always be exclusively relied upon. Primary ores may extend downward indefinitely and may fluctuate in value independently of depth: if primary ores are consistently lean for a considerable vertical distance, there is little reason to expect that, still deeper, they will increase to the commercial grade; on the other hand, rich primary ores may persist uninterruptedly downward or may come in again below a lean interval. Secondary ores, however, have a comparatively limited vertical extent; in a large way enrichment decreases with depth and finally gives out. It follows then, that when a hole descends from profitable ore into ore of less than the commercial minimum, the practical significance of the situation depends upon whether this decrease results from a decrease in secondary enrichment or is a variation in primary content: if the copper of the ore passed through has been chiefly secondary, little is gained in the average case by extending the hole much below the point at which the commercial limit is reached; but, when copper is chiefly primary, due weight must be given to the possibility that, still deeper, the ore may again improve. The distinction between primary and secondary ore may of course be effected through an examination of the drillings. It has been found, however, to be facilitated by curves made by plotting assays against

Jan 1, 1916

By E. T. Turkdogan, P. Grieveson, J. F. Beisler

Experimental results are given for the rate of reduction of silica from silicate melts by paphite-saturated iron in the presence of carbon monoxide. It is shown that, when gas bubbles are present at the slag-metal interface, the interfacial chemical reaction is the rate-controlling process in the transfer of silicon from slag to metal. From the silicon-concentration profiles in the metal sample, the diffusivity of silicon in paphite-saturated iron is found to be (5.4 * 0.4) x 10 sq cm per sec at 1600°C. Some consideration is given to the transport of oxygen from the slug-metal interface to the walls of the gvaphite metal container as becoming the rate-controlling process in the absence of gas bubbles at the slag-metal interface. ATTEMPTS were made by Fulton and chipman1 to investigate the kinetics of reduction of silica from calcium alumino-silicate melts by graphite-saturated iron in an atmosphere of carbon monoxide. In these experiments with 400 to 500 g of metal and slag, both phases were stirred in such a manner that the interface was essentially undisturbed. Initially, the graphite-saturated iron contained about 15 pct Si and, after about 8 or 10 hr of reaction time at 1600°C, the silicon content of the metal in- creased by about 0.2 pct. In a written discussion on this paper of Fulton and Chipman, schuhmann2 pointed out the possibility that this observed slowness of the reduction of silica could be due to the transport of oxygen across the liquid metal boundary layer at the slag-metal interface. Although this explanation of Schuhmann is quite feasible for the experimental data of Fulton and Chipman on silica reduction, such a reasoning should not be extended to other rate data on slag-metal reactions unless sufficient evidence is available satisfying the boundary conditions for such a transport process. The hydrodynamics of stirred liquids are very complex and even for a simple method of stirring there is no exact mathematical solution which will predict the mass transfer coefficient accurately. The best available solution of this problem is that given by Lewis' and later modified by mayers~ for a two-liquid system where liquids are stirred by counter-rotating stirrer blades without disturbing the interface. In such a system the mass transfer coefficient is estimated from an empirical relationship using the data on viscosity and density of the two liquids, rate of revolution, the length of stirrer blades, and the diffusivity of the element which is transferred from one phase to the other. It was found in these investigations' that the estimated and observed mass transfer coefficients, in systems containing two immiscible aqueous solutions, agreed within *40 pct. Although this is not considered to be an unreasonable error for the study of industrial processes, uncertainties of this magnitude cannot be tolerated in any theoretical study of reaction kinetics. In view of the complexity of the

Jan 1, 1963

By A. G. H. Anderson, Eric R. Jette

During the period from 1910 to 1920, there was a lively interest in the subject of grain growth and many papers were published, followed by interesting discussions. Questions dealing with the fundamentals of grain growth—why and how it occurs—were treated in papers by Howe,' .Jeffries,² Sauveur,² Chappell,4 Beilby,5 Mathewson and Phillips,6 Mc Adam,7 Carpenter and Elam,8 Stead and Carpenter,9 Ruder,l0 as well as others. Since that decade, much indeed has been done regarding the practical control of grain size, and it is now possible to order material having a size sperified in the American Society for Testing Materials classification. Also, one hears the term "spliced boundaries" used in connection with certain tungsten lamp filamentsl1 wherein it is important to prevent "sagging" between consecutive turns of the helix.12 This practical use of a certain knowledge as to the things that influence or even control grain growth should not be taken as an indication that the subject has been thoroughly explored and that nothing more can be learned from fundamental studies. It is with this thought in mind that a report of some observations and experiments on abnormal grain growth is believed justified. Abnormal grain growth is met with in heat-treating high-carbon steels in the austenitic range,'? in the hardening treatments of high-speed steels,14'15 and in the low-temperature annealing of strained low-carbon steels as in sheet and wire material. Entirely aside from these instances of exaggerated grain growth, which some might consider as freakish, it is thought that abnormal growth is simply a case where the growth forces and the forces tending to prevent growth are almost, but not quite, evenly balanced. Information relative to grain-growth characteristics in general may be obtained from a study of abnormal growth conditions, which may be looked upon as vantage points. Reflection will show at once that if growth forces are great in comparison to inertia or resistance to growth, many crystals start to grow and, for that reason, none becomes very large, whereas if inertia is

Jan 1, 1938

By Eric R. Jette, A. G. H. Anderson

During the period from 1910 to 1920, there was a lively interest in the subject of grain growth and many papers were published, followed by interesting discussions. Questions dealing with the fundamentals of grain growth—why and how it occurs—were treated in papers by Howe,' .Jeffries,² Sauveur,² Chappell,4 Beilby,5 Mathewson and Phillips,6 Mc Adam,7 Carpenter and Elam,8 Stead and Carpenter,9 Ruder,l0 as well as others. Since that decade, much indeed has been done regarding the practical control of grain size, and it is now possible to order material having a size sperified in the American Society for Testing Materials classification. Also, one hears the term "spliced boundaries" used in connection with certain tungsten lamp filamentsl1 wherein it is important to prevent "sagging" between consecutive turns of the helix.12 This practical use of a certain knowledge as to the things that influence or even control grain growth should not be taken as an indication that the subject has been thoroughly explored and that nothing more can be learned from fundamental studies. It is with this thought in mind that a report of some observations and experiments on abnormal grain growth is believed justified. Abnormal grain growth is met with in heat-treating high-carbon steels in the austenitic range,'? in the hardening treatments of high-speed steels,14'15 and in the low-temperature annealing of strained low-carbon steels as in sheet and wire material. Entirely aside from these instances of exaggerated grain growth, which some might consider as freakish, it is thought that abnormal growth is simply a case where the growth forces and the forces tending to prevent growth are almost, but not quite, evenly balanced. Information relative to grain-growth characteristics in general may be obtained from a study of abnormal growth conditions, which may be looked upon as vantage points. Reflection will show at once that if growth forces are great in comparison to inertia or resistance to growth, many crystals start to grow and, for that reason, none becomes very large, whereas if inertia is

Jan 1, 1938

By W. S. Landis

In brief, this is the story of an attempt to Americanize a process originally developed in Europe. The story will be recited in two sections, the first dealing with the process as developed by the European engineers; the second containing the improvements and modifications of American origin, together with some details of the operating results of the unit as finally assembled. Developments in other directions in this same field have not, up to the present, pointed out an economic future for the process, therefore our record here is largely a report of development progress. Whether some particularly favorable location will be found at some future time for a commercial installation cannot as yet be foretold. The project is now at a standstill. The peculiar tools of the electrometallurgist should be of great interest to the zinc smelter. The low thermal efficiency of the zinc retort, its comparatively small-scale unit and its intermittent cycle as it stood in 1925, should make this art a particularly fertile field for the electric furnace. Yet in spite of years of work recorded in volumes of literature, and an expenditure of large sums of money, there is not a single electrothermic zinc smelter operating anywhere in the world. In this industry the electric furnace plays only a secondary part today. Historical The first serious proposal to use the electric furnace for the smelting of zinc ores was made by the Cowles Brothers in 1885, but their experimental work did not advance the art to any extent. The next investigator of this field was Dr. Gustav DeLaval, a Swedish engineer well known to the industrial world through his development of the centrifugal and the steam turbine. The DeLaval cream separator is a familiar household appliance in most parts of the world. Although Dr. DeLaval commenced his experiments in the field of electric zinc smelting in 1893, it was not until 1898 that he had a practicable furnace, even then operating but intermittently. His work was done at Trollhättan, Sweden. He continued to improve this early fur-

Jan 1, 1937

By R. S. Archer

In the microscopic examination of aircraft-engine parts made of heat-treated alloy steels, the writer has been forcibly impressed by the failure of the usual etching processes to disclose any but gross defects in heat treatment. It seemed particularly desirable to bring out the grain size of the steel, which is indicated in the ordinary etching processes chiefly by the change in orientation of structure from grain to grain. After various attempts, a fairly successful method has been found, which is here presented in the hope that it may be of use to those who have occasion to examine these steels in the hcat-treated condition. The specimens worked with have been mostly chrome-nickel steels heat treated (that is, hardened and tempered) to a Brinell hardness of around 300. A few experiments with other specimens will be referred to later. Briefly, the method employed consists in etching the steel about 10 min. in a fresh solution of picric acid in ethyl alcohol, and then rubbing off the smudge of carbonaceous matter on moist broadcloth. Different samples of almost identical analysis, heat treatment, and physical properties (including resistance to impact) respond quite differently to this treatment. In some, the grain boundaries are developed quite readily, while in others, especially in those whose grain is unusually fine or in which the final hardening heat has not quite obliterated the previous crystallization, the results are more obscure. The exact time of etching to secure the best results also differs for various samples, and the greatest success is usually attained by a process of "tinkering." Such a process is illustrated in a series of micrographs, the first six of which were taken at a magnification of 300 diameters. The properties of the steel are as follows: Carbon, per cent............... 0.42 Brinell hardness.............. 293 Nickel, per cent................ 1.35 Yield point, pounds per square Chromium, per cent............. 0.90 inch........................ 131,000 Copper, per cent................ 0.025 Maximum strength, pounds per Manganese, per cent............ 0.74 square inch................. 144,500 Phosphorus, per cent............ 0.024 Elongation in 1 in., per cent... 28 Sulfur, per cent................ 0.036 Lod impact, foot-pounds...... 51 Reduction of area, per cent...... 57.3

Jan 1, 1920

By W. O. Philbrook, H. W. Hosking, N. B. Melcher

A simple and inexpensive mercury-tracer method has been develohed to study rates and Patterns of gas flow in blast furnaces. A Pulse of mercury is injected into the hot blast, and its arrival at the sampling Point is recorded by an electronic circuit that measures resonant absorbtion of ultraviolet light by mercury vapor in the gas aspirated .through the detecting. cell. A rapidly developing interest in blast-furnace technology in recent years has created a strong demand for precise knowledge of the rates and patterns of gas movement through the stock column. Classical fluid-flow theory cannot supply the desired information because the complexity of the blast-furnace situation precludes the accurate determination of many of the parameters required for solution of the equations. In fact some of the terms employed in fluid-flow treatments become almost meaningless under blast-furnace conditions. The void fraction of the stock column, for example, varies widely from place to place and is affected by the segregation of charge materials, attrition of lumps during descent, and channeling. Gas density varies with changes in local pressure, temperature, and composition, while viscosity varies with temperature and composition. Even if mean values for these functions were acceptable, they would be either impossible or extremely difficult to determine with a high degree of accuracy since the value of the mean for all gas properties would depend upon the flow distribution itself. Attempts to study gas movement by the pitot-tube determination of kinetic pressures have met with little acceptance. Reproducibility of results is extremely difficult to achieve in a situation where alignment of the tube orifice with respect to the flow direction in tortuous channels cannot be guaranteed. Because of these difficulties it would appear that progress can be achieved only with a direct method of measuring gas velocities and determining the shape of flow paths through the stock. The establishment of such a method is described in this paper. SELECTION OF METHOD Direct measurement suggests the use of a tracer by means of which the progress of a "parcel" of gas can be followed through the furnace. Several requirements must be met before any selected material can be considered a suitable tracer. First of all, it must be a substance not normally present in blastfurnace gas or dust; otherwise its presence in a gas sample will have little significance. It should be volatile at temperatures normally existing within the furnace, to ensure that it will travel with the gas, as a gas. It should possess special properties enabling its presence in the gas to be detected readily, and it should not undergo exchange reactions with any material normally present within the furnace, including refractories and coke as well as all components of the metal and slag. Radioactive materials naturally are considered because their radioactivity renders them susceptible to detection. However, of the many radioactive materials available, almost all are eliminated from final consideration by their unsuitability in terms of other properties. Radioactive silicon, carbon, calcium, phosphorus, and many others have been considered and discarded, either because they are not volatile over the whole range of significant temperatures, or because they could be expected to undergo exchange reactions with burden or refractory materials. Others which might be suitable in terms of these properties are eliminated because of a low activity, short half life, or the necessity for fragile counting apparatus. Of the many elements available in radioactive form, perhaps radon is the only one suitable for blast-furnace gas-flow studies. This has been used in several investigations1-4 with considerable success. The use of radiotracers has certain inherent disadvantages. One is the cost. An appreciable sum must be allowed for materials each time a test is made. Also, special methods of handling must be employed, and very often the progress of an investigation must be governed by the availability of isotopes and the delivery arrangements that can be made for them. An advantage is immediately gained if the tracer material can be a substance which can

Jan 1, 1960

By G. S. Tint, M. Herman, V. V. Damiano

Dislocation arrays and substructures were studied in cadmium doped zinc crystals using a newly devised etching technique. Cadmium precipitates delineating the dislocations were revealed by etching a surface closely parallel to the (0001) slip plane. Cinephotomicrography of the continuous etching process revealed the three-dimensional aspects of dislocations in the bulk crystal. Dislocation etch patterns were studied in both deformed and annealed crystals after suitable aging at room temperature. The effect of annealing was evidenced by a rearrangement of the dislocations into low-angle boundaries and hexagonal networks. ETCH pit techniques have been used extensively to study dislocations in both deformed and annealed bulk metal crystals. Ideally one hopes to obtain a one-to-one correspondence between the etch pits and the points of emergence of the dislocations at the surface. One then attempts to deduce the way in which dislocations are arranged in the bulk crystal from the arrangement of etch pits on the surface. It is clear that one can obtain only limited information of the dislocation configurations inside the crystal from etch pit studies of single surfaces. Considerably more information is obtained if one is able to follow the course of the dislocations through the crystal using progressive etching technique. Techniques of this sort were used by Gilmanl to study dislocations on the slip planes of NaCl crystals and by Damiano and Tint2 to study dislocation arrangement in zinc crystals grown from the melt. The present paper makes use of a technique first described by Tint and Damiano3 to observe and continuously record the dislocation structures which appear while a crystal surface was being progressively etched. Studies were made on cleaved (0001) surfaces to reveal the dislocations along their length on the surface closely parallel to the slip plane. The technique for revealing segments of dislocations along their length by etching is well known. Wilsdorf and Kuhlmann-wilsdorf4 revealed disloca- tions along their length in aluminum containing a few percent copper, when precipitates segregated along the dislocations. The technique was used by Low and Guard5 to study dislocation configurations on the slip plane in Fe-Si alloys containing carbon. In the present work the technique was applied to zinc containing cadmium since it was shown by Gil-man6 that a cadmium-rich phase could be made to precipitate from supersaturated solutions along dislocations in zinc. Segments of dislocations delineated by the precipitates were revealed by etching a surface prepared by cleaving the crystal. The three-dimensional nature of dislocations and substructures was thus studied from the cinephotomicro-graphic record of the continuous etching process. EXPERIMENTAL Single crystals of zinc containing the order of 0.1 pct Cd were prepared by slowly lowering a graphite crucible containing the melt through a temperature gradient of 15°C per cm at a rate of 1.5 X 10-3 cm per sec. "As grown" crystals were aged for periods of 1 month at room temperature, then cleaved in liquid nitrogen, and etched according to the procedure used by Gilman.' The etchant containing 32 g of CrO3, 6 g of hydrated Na2SO3 in 100 ml of water behaved as a chemical polish for zinc and etch pits were produced at the site of precipitates or inclusions. After the precipitates or inclusions were removed from the surface, the etch pits left behind were eventually polished smooth. This behavior enabled one to continuously observe the surface while the specimen was immersed in the etchant. Best results were obtained when the specimen surface was vertical and the reaction products of polishing were continuously removed by gravitational convection. Some crystals were heavily deformed in excess of 25 pct strain, others were lightly deformed the order of a few pct by compression such that the deformation occurred essentially by basal glide. Some crystals were etched immediately after deformation, others were allowed to age at room temperature for several weeks prior to etching. Heavily deformed crystals were annealed at various temperatures and etched on the cleavage plane immediately after annealing, others were allowed to age at room temperature for several weeks prior to etching. The etched structures of deformed and annealed structures were studied. Similar experiments were conducted on 99.9999 pct pure zone refined Tadanac zinc crystals which

Jan 1, 1963