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By C. M. Schwartz, A. E. Austin, W. B. Wilson

High-temperature X-ray diffraction studies were conducted with Th-U alloys with up to 10 wt pet U. The solid solubility of uranium in thorium as a function of temperature was determined by the method of lattice parameters. Thorium will dissolve up to 2.5 wt pet U at 950°, 4.5 wt pet U at 1150°, and 7.5 wt pet U at 1250°C. Determinations were made of the temperature of the transition of thorium and of the effect of uranium upon the transition. The a to ß transition for thorium was observed to occur at 1330' ±20°C. Mean coefficients of expansion were calculated for thorium and two alloys, and for ThO2 in contact with the thorium, using X-ray lattice-parameter data. Values obtained at 950° C for thorium and Tho2 were 12.1 and 9.40 X 10-6 per OC, respectively. Impurities obtained during the X-ray exposure were identified by diffraction and were essentially Tho2 and ThC, with two additional unknown phases being detected. The effect of the impurities upon the results is discussed. DIRECT investigation (i.e., high-temperature X-ray diffraction studies) of the phase diagram of thorium-rich uranium alloys has been shown to be necessary since recent work1 - has disclosed the presence of an allotropic transformation near 1400°C in pure thorium with the room temperature face-centered-cubic phase transforming to a body-cen-tered-cubic structure at the elevated temperature. The effect upon the transition of the addition of uranium to thorium and of the solubility of uranium in thorium at high temperatures remained unknown, yet was of interest in understanding fabrication procedures and elevated temperature use. The present work was undertaken to provide information in this area by determining the transition temperature, the effect of uranium on the transition temperature, and the solubility of uranium in thorium as a function of temperature. Experimental Work The high-temperature diffraction data were obtained using a camera especially designed for the purpose3 and capable of reaching temperatures in excess of 2000°C at pressures as low as 1 x 10." mm Hg. Temperature regulation was provided by regulating the power input to ±0.1 pet variation, and by regulating the water flow through the camera jacket to provide a constant thermal load. The X-ray sample was a rod nominally 80 mil diam, which was further turned down to 20 mil and then etched to 18 mil over 1/2 in. of one end. This was placed in the sample holder and mounted on the camera so that the smaller part was surrounded by a cylindrical tantalum-sheet radiation-type heating element. Diffraction from the sample was recorded on film after passing through a slot in the heating element and radiation-baffle shield and through beryllium vacuum windows. The X-ray film mounting was of the Straumanis type4 with a camera diameter of 114.59 mm. Since previous work of Chiotti' indicated that impurities considerably alter the transition temperature, chemical analysis of the arc melted iodide crystal-bar thorium samples was obtained prior to testing. The analysis disclosed the material to contain as low as 0.001 ±0,0002 wt pet H and 0.007 ±0.001 wt pet 0. Carbon was 0.003 wt pet and nitrogen less than 0.002 wt pet. This material was sealed in mild steel in an inert atmosphere and subsequently hot rolled to 3/8-in. diam rods at a temperature of 732°C. Following removal of the jacket, the material was pickled and cold swaged to 1/8-in. rods, from which the diffraction samples were prepared. The alloys were similarly prepared, with the uranium being added during arc melting. The uranium analyses of the alloys prepared appear in Table I. The experimental procedure for diffraction examination of the three samples of high-purity thorium differed from those of the Th-U alloys. The original practice, later modified, consisted of pumping down the camera with the diffusion pump on and then admitting liquid nitrogen to the cold trap of the system. This was modified for the Th-U alloys by maintaining liquid nitrogen in the cold trap at all times before and while the diffusion pump was heated. This minor change produced a reduction in the amount of carbon pickup by the sample during exposure to the diffusion-pump vapors. The sample was brought to the desired test temperature and exposed for 21/2 hr at pressures which were usually 2 x 10-6 mm Hg, or lower. Exposures were made at

Jan 1, 1959

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 J. E. Hilliard, J. W. Cahn

calculation has been made of the standard deviations to be expected in the measurement of volume fractions by areal analysis, lineal analysis and four point-counting Procedures. The effect of experimetztal errors is not included. Our conclusion is that a point count using a two-dimensional grid will be the most efficient method of volume fraction analvsis providing the grid spacing IS coarse enough. The predicted standard deviation for such an analysis is shown to he in good agreement with that determined experimentally. A metallurgist wishing to estimate a structural property by means of quantitative metallography is often faced with a choice between several different procedures. In such a case, he will naturally wish to know: a) Which procedure is the most efficient in the sense of requiring the least effort for a given precision? b) For a given procedure, what are the conditions for maximum efficiency? c) Under these conditions, how many measurements are required to attain a given precision? It is our aim in this paper to provide at least partial answers to these queries as they relate to the estimation of volume fractions from measurements on a random two-dimensional section of an opaque specimen. The commonly used techniques1,2 for volume-fraction analyses are based on one or more of the following principles: i) For an areal or Delesse3 analysis: That the areal fraction of a three-dimensional feature intercepted by a random plane provides an unbiased estimate of the volume fraction of that feature. ii) For a lineal or Rosiwal4 analysis: That the fractional intercept on a line passing at random through a two-or three-dimensional feature provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. iii) For a point-count analysis: That the fractional number of randomly or regularly dispersed points falling within the boundaries of a two-dimensional feature on a plane, or within the boundaries of a three-dimensional feature in a volume, provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. The absence of bias referred to in these principles does not, of course, imply that the results of an analysis will be free of error, but only that the expected result is equal to the true one. Application of the foregoing principles provide the following six possible experimental procedures: a) An Areal Analysis—This involves the measurement with a planimeter (or other means) of the area of a constitutent intercepted by the plane of polish b) A Two-Dimensional Random Point Count—Apos-sible experimental procedure for this analysis is to superimpose a sheet of transparent graph paper on a micrograph, and then use a table of random numbers to select coordinates for the points. c) A Two-Dimensiotuzl Systematic Point Count-Similar to b) except that the points are distributed in a prescribed manner, usually at the corners of a lattice superimposed on a micrograph or the screen of a projection microscope. d)A Lineal Analysis—A measurement of the fractional line length intercepted. It is usually performed by traversing the specimen under the cross hairs of a microscope and recording the distance travelled in each constituent. e) 4 One-Dimensional Random-Point Count— This could be performed by traversing the specimen with stops at random intervals to identify the constituent then present under the cross hairs. f) A One-Dimensionul Systematic Point Count— Similar to e) except that the traverse is stopped at prescribed (usually equal) intervals. It will be noted that the point-counting procedures b) and c) can be regarded as methods of estimating the areal fraction. Similarly, e) and f) are indirect methods of making a lineal analysis. All of the six procedures described above involve at least one stage of sampling. Thus, quite apart from any experimental errors, there will always be a statistical uncertainty associated with the final results. It is with the calculation of this uncertainty that we will be concerned. To avoid unnecessary repetition, the statistical relationships that will be used in the calculations are collected together in the appendix. For a fuller discussion reference should be made to one of the many textbooks5,6 on statistics. For symbols relating to the specimen structure we will follow as far as possible the terminology used by Smith and Guttman.7

Jan 1, 1962

By J. W. Snavely

WITH all the advantages of handling bulk materials by means of belt conveyor also go some problems, one of the most persistent being that of cleaning. When sticky materials are being carried; the build-up of material on the return idler rolls results in difficulty of belt training. Much attention has been given to the problem of cleaning conveyor belts, and a great variety of cleaning devices have been developed. Even the best involve troublesome maintenance, and none can completely remove the fine particles imbedded in the belt cover, which cause rapid wear of the return idler rolls, and at the same time, of the belt cover as well. One of the major rubber companies has been promoting a two-way belt system, in which the conveyor belt is given two successive 90" twists at each end to enable it to carry material in both directions simultaneously. For many years the flat belt transmission industry has installed quarter-turn and half-turn twists in countless numbers of instances. While quarter-turn and half-turn twists in transmission belts is a familiar application, the 180" twist apparently has never been previously attempted with a conveyor belt. About a year ago, two officials of the National Iron Co. of Duluth, Lester and Lewis Erickson, proposed twisting the return run of a conveyor belt on an installation that they were designing for one of the major iron ore producers. Since then the soundness of the idea has been demonstrated, both in theory and by practical test, with the result that the installation of two conveyor belts involving the twisting of the return run is now under way. These two installations are designed to have the return run of the conveyor belt twisted 180" as it leaves the snub pulley at the head drive. The clean underside of the belt is thus placed against the idlers on the return run as well as on the carrying run. Just before it enters the tail pulley, the belt will be twisted an additional 180°, restoring it to its normal position. Because this twisting of the return run of a conveyor belt is a radical departure from accepted practice, an elaborate and extensive test was conducted early in 1950 to demonstrate that this twisting of the return run could be done successfully, also to establish application data for accomplishing this twisting, and to determine if any special equipment would be required. In studying this concept of twisting the return run of a conveyor belt, a number of problems need to be solved, primarily the ones brought about by deliberately introducing an unequal distribution of stress across the conveyor belt and controlling that maldistribution of stress, while confining it to the return run portion. The tension conditions existing in the return run of a conveyor belt are clear to all designers. First, the return run carries the initial or slack side tension of the conveyor belt, the tension that must be supplied to the return run to provide proper frictional contact between the belt and the driving pulley so that the necessary power can be transmitted from the driving pulley to the belt without slippage. This slack side tension is supplied to the belt by means of takeups, either of the gravity type, which can be vertical or horizontal, or by means of the screw type. With inclined or declined belt conveyors the slope tension also must be considered, which is the tension imposed by the weight of the belt hanging from the top pulley. This slope tension frequently can furnish part or even all of the initial tension required. The maximum value of the slope tension will be at the top pulley, and it decreases in direct proportion to the length. In addition to the foregoing, it frequently is desirable to impose arbitrarily additional slack side tension to provide sufficient tension at the loading point at the tail, so that the belt will adequately support its load between the carrying idlers. Design Conditions for Twisting A number of design conditions exist, which must be satisfied successfully to accomplish the twisting of the return run without exceeding normal working limits in any portion of the conveyor belt. It is obvious that the belt edge, in its relation to the center of the belt, must stretch in making a twist, because as the twist is accomplished, the belt edge travels through a longer path than does the center of the belt. It is further obvious that if the edge of the belt is stretched, a redistribution of stress in the belt is required to allow this edge stretching. Moreover, this stress will be unequal across the width of the belt, having a maximum value at the edges, with a minimum value at the- center of the belt. With correct initial tension in the return run of a conveyor belt, the existing slack side tension will be unequally distributed when a twist is introduced. A condition then exists in which the edge stresses,

Jan 1, 1952

By William D. Klopp

A study was conducted of the tensile and creep properties of are-melted and electron-beam-melted tungsten over the temperature range 2250° to 4140°F. The tensile and creep strengths vary with pain size, the finer -grained materials being stronger. The activation energy for transient creep at 2250° to 3500°F is 95,000 cal per (g)(mole), while that for steady creep at 3300o to 4000°F is 141,000 cal per (g)(mole). At 2875o to 3300°F the apparent activation energy for steady creep decreased with decreasing temperature. It is suggested that cross slip is rate controlling during transient creep, while dislocation climb is rate controlling during steady creep above 3300° F. ALTHOUGH considerable data have been generated on the high-temperature tensile properties of powder-metallurgy tungsten,1 relative few data have been published on the properties of are-melted2 or electron-beam melted tungsten.3 Furthermore, the available data show a fairly large amount of scatter at high temperatures. The effects of structure and purity have not yet been defined, aside from observations that high-purity electron-beam (EB)-melted tungsten3 and single-crystal-plasma-flame tungsten4 are weaker than less pure powder-metallurgy tungsten. The creep behavior of powder-metallurgy tungsten has been studied, but no data are available on the creep behavior of tungsten consolidated by melting. Green5 found that powder-metallurgy tungsten exhibited linear creep at 4082° to 5072°F with an activation energy of 160,000 cal per (g) (mole). The similarity of this activation energy to that of 153,000 cal per (g)(mole) for volume self-diffusion6 suggests that recovery of strain hardening by dislocation climb is rate controlling in this temperature range. In studies at 4800°F, Sutherland and Klopp7 concluded that grain size significantly affected the creep behavior of commercial powder-metallurgy materials. This grain-size effect was suggested by sherby,8 although the opposite relation had been reported for aluminum.' The purpose of the present study was twofold: first, to provide baseline data on high-temperature tensile and creep properties of are-melted and EB-melted tungsten for concurrent tungsten alloy studies, and, second, to determine the phenomenolo-gical effects of structural and purity variables on the high - temperature mechanical properties of tungsten. EXPERIMENTAL The are-melted tungsten materials were prepared by melting sintered 1-1/4-in.-diam electrodes into 2-1/2-in.-diam by 5-in.-long ingots. The are-melting facility has been described previously.' Eight ingots were melted, machined, and hot-extruded at

Jan 1, 1965

By J. L. Lamont, W. Crafts

Studies of the effect of composition of steel on hardenability by Grossmann,' and as-quenched hardness by Field2 and by the authors, have made it possible to predict the results of quenching when the composition and cooling rate are known In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tem-pred properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq, in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as-quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content. Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after like heat-treatment, differ considerably in tensile strength. Procedure In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08 to 0'65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc' The accuracy of the method was finally checked on a variety of carbon, low-alloy and high-alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from 1/2 to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability speci-menS quenched from a normal temperature for austenitizatios were used to obtain a range of as-quenched Rockwell C

Jan 1, 1948

By W. Crafts, J. L. Lamont

Studies of the effect of composition of steel on hardenability by Grossmann,' and as-quenched hardness by Field2 and by the authors, have made it possible to predict the results of quenching when the composition and cooling rate are known In order to extend the application of the hardenability calculation to the quenched and tempered condition in which steel is finally used, a survey has been made of the hardness changes caused by tempering. From this study a method has been developed for the prediction of hardness and tensile strength of steel in the tempered condition. The method of calculation was developed from Rockwell C hardness tests on quenched and tempered Jominy specimens and is expressed in Rockwell C hardness units. It is of an additive type in which the degree of softening from as-quenched hardness is estimated. Tem-pred properties may be calculated within about plus or minus 5 Rockwell C hardness or plus or minus 15,000 lb. per sq, in. tensile strength. This degree of accuracy is less than that necessary for the control of heat-treatment, but is adequate for the comparative evaluation and selection of alloy steels. The formula indicates that tempered hardness is primarily dependent on as-quenched hardness and, as in the hardening reaction, the progress of tempering is controlled mainly by the carbon content. Alloys tend to retard softening by a secondary hardening mechanism in which the alloy appears to migrate from ferrite to the carbide phase. The factors for the effects of alloys in tempering vary so much from the effects of alloys in hardening that different steels of equivalent hardenability may, after like heat-treatment, differ considerably in tensile strength. Procedure In developing the method for calculating tempered Rockwell C hardness, simple and complex steels were tested over a range from 0.08 to 0'65 per cent carbon and up to 2.68 per cent manganese, 2.18 silicon, 3.50 chromium, 4.94 nickel, and 1.06 molybdenum. The steels were made as small induction-furnace heats at the Union Carbide and Carbon Research Laboratories, Inc' The accuracy of the method was finally checked on a variety of carbon, low-alloy and high-alloy types of heat-treating steels produced under commercial conditions. The method was based on a study of tempered Jominy bars, and its validity was tested by correlation with the center hardness and tensile strength of oil-quenched and tempered bars from 1/2 to 4 in. in diameter. The method of calculation was derived from the differences in Rockwell C hardness between as-quenched and quenched and tempered Jominy specimens. Prenormalized Jominy hardenability speci-menS quenched from a normal temperature for austenitizatios were used to obtain a range of as-quenched Rockwell C

Jan 1, 1948

By Jesse O. Betterton, Y. E. Lebedeff

AS a matter of the most widespread interest to lead-refining metallurgists, the process of desilverizing lead originated by Parkes is the most fundamental step in lead refining. While this basic operation, in addition to effecting a practically complete recovery of gold and silver, is also a great purifying operation and a governor on the purity and uniformity of the final refined lead, it has the important deficiency that no bismuth is removed in the operation. The problem of finding a satisfactory, inexpensive method for removal of bismuth that would fit in with the basic desilverization step has been one of enticing interest for lead-refinery metallurgists for many years. Of late it has become one of imperative interest, and while many attempts and much progress have been made, it is probably fair to say that metallurgical progress thus far is only catching up with commercial requirements. The Pattinson process, an original competitor of the Parkes process for desilverization, has received much attention for its possibilities for bismuth removal. Bismuth concentrations in the Pattinson process fall far short of the silver concentrations and as a result too many operations are required and a crawl in grade in the kettle units is experienced which requires periodic correction. Altogether, it has proved too expensive a remedy, from the cost standpoint of both installation and operation. The Betts electrolytic process is a fully satisfactory remedy but its present status in the field of lead refining is more a matter of bismuth removal than preference as a refining system, except, of course, in instances particularly favorable to the basic requirements of the process. The Betts process, of course, is essentially different from the Parkes process, and very difficult to associate therewith to any economy except in minor ways. Accordingly, where economy dictates the Parkes process, and this is true of far the greater portion of the world's tonnage, the adoption of the Betts process primarily for bismuth removal is apt to prove an expensive remedy on account of its normally higher cost of operation, inelasticity of the equipment for variable tonnages, and high per ton cost of installation.

Jan 1, 1937

By T. V. Falkie, D. R. Mitchell

Many operational problems in mine haulage cannot be solved economically by conventional analytic or trial and error methods. However, a method of probabilistic simulation, which is based on the fundamental assumption that many of the variables governing any physical system are probabilistic, has been adapted to certain areas of operations research in coal mine haulage. This paper attempts to illustrate how simulation can be used in basic haulage research and what kind of results can be expected. Optimization in this case is performed in terms of locomotive and car movement, as well as best utilization of men and equipment, and is approached primarily from the standpoint of scheduling of the main haulage. Many operational problems in mine haulage cannot be solved economically by conventional analytic or trial-error methods. However, a method of probabilistic simulation, which is based on the fundamental assumption that many of the variables governing any physical system are probabilistic, has been adapted to certain areas of operations research in mine haulage. In many physical cases several probability distributions interact with each other in special ways, and it is not possible to solve for their combined effect in a mathematical equation. This is often true in the case of mine haulage, where such variables as number of empties or loads per trip, travel times, and number of cars or tons produced in a given time are probabilistic. By using a simple example of one secondary haulage segment of a large underground haulage system, this paper attempts to illustrate how simulation can be used in basic haulage research and what kind of results can be expected. Optimization in this case is performed in terms of locomotive and car movement, as well as best utilization of men and equipment. This is the type of preliminary research that will be needed as a first phase in any major haulage study, whether it be a relatively simple economic analysis or a plan for complete automation. The problem of optimization has been approached primarily from the standpoint of scheduling of the main haulage. It is evident that the method of proba-

Jan 1, 1963

By Robert H. Hafner, Irvin R. Kramer, Stewart L. Toleman

IN his paper on the calculation of hardenability from chemical composition, Grossmann1 discussed the effect of most of the alloying elements used commercially. The purpose of the work reported in this paper was to determine the effect of several other elements on hardenability-arsenic, antimony, beryllium, cobalt, columbium, germanium, tellurium, tin, aluminum, and titanium-and to extend the range of composition of some of the elements studied by , Grossmann-chromium, copper, manganese, molybdenum, nickel and silicon. EXPERIMENTAL METHODS To determine the effect on hardenability, suitable amounts of the alloying elements were added to experimental heats and the hardenability determined by means of end-quenched hardenability specimens. The steels were melted in a high-frequency induction furnace with a basic crucible, using ingot iron as a base for some of the heats and S.A.E. 1015 for others. The alloying additions were made as ferroalloys or as metal, depending on the ' alloying element. Hundred-pound heats were split and poured into square, tapered, cast-iron ingot molds with hot tops. Aluminum was not used as a deoxidizer in most of the heats. The ingots were homogenized for 12 hr. at 1260°C. (2300°F.) , and forged into rounds of 1 ½ in. diameter. These bars were normalized twice from 840°C. (1550°F.) before machining into Jominy bars. The composition of the steels was deter- [ ] mined in most cases by samples taken from the end-quench hardenability specimen. As suggested by crafts,2acid-soluble

Jan 1, 1943

By Magnus Troilius

SINCE the discussion on steel rails in America has forcibly drawn attention to the value of chemical analysis, if not as a necessary stipulation, at least as a guide to control the usual mechanical tests, some doubt has been thrown upon the accuracy of the analytical results obtained by different chemists. To any one having the least acquaintance with chemistry, it is quite clear that if exactly similar results are to be obtained from the same borings of steel, exactly the same methods must be used by the different analysts. Hence the necessity (if complications are to be avoided) of establishing what I may call standard or normal methods, to be used both by the inspectors and by the chemists at the works. Remembering that the application of chemistry to steelrail inspection is yet in its infancy, it is of great importance to possess a perfect acquaintance with the best methods in use. Being myself a grateful pupil of Professor Eggertz, of the School of Mines in Sweden, it occurred to me, two years ago, that I could not do better than start a laboratory of my own, and engage one of his pupils, Mr. Troilius, for the purpose of analyzing the steel borings from mechanically-tested rails, so that I might thus obtain without delay thoroughly accurate determinations. Moreover, in order to carry on the operations in perfect accordance with the methods used at the steel works in England and Germany, where I had to control the manufacture, I deemed it desirable to allow Mr. Troilius to go through a course of training at these works; and I gladly seize this opportunity of expressing my grateful acknowledgments to several works in England and in Germany for affording every facility for such an exchange of information as mas found necessary in arriving at the best analytical methods to be used.

Jan 1, 1882

[VOL. XXXVI. Page. Line. 155 29 For "Joachimstahl," read "Joachimsthal." 215 Foot-note 2. For " May, 1892," read " May, 1902." 216 21 For " ack-screw," read " jack-screw." VOL. XXXVII. 31 3 For "quantity of tons," read "quantity of slimes." 35 10 Expunge "recorded in Table VII." 37 24 Expunge "to." 38 33 For "page 89," read "page 9." 44 40 For "page 86," read "page 6." 47 In table, third line under heading "Excavators and Conveyors," expunge "per 40 ft. of."]

Jan 1, 1918

By L. S. Darken

IT has been known for sometime that in an ionic lattice, such as that of Ag2S or FeO, the migration velocity of the anion may differ markedly from that of the cation, the cation being usually the more mobile. It has been shown, for example, that during the formation of silver sulfide tarnish on silver, the tarnish layer grows principally by the motion of silver cations through an essentially stationary silver sulfide lattice. Similarly, the growth of wüstite scale on iron proceeds principally by motion of iron ions, this being accomplished with the aid of vacant iron lattice sites into which the iron may readily move. Likewise investigations of solid solutions of various salts show that there is usually considerable difference in the mobility of the different cations. Measurements of the mobility of various metals in liquid mercury indicate that the various metals move at different rates relative to the mercury. In view of the foregoing it seems reasonable to suppose that when any single phase solution is acted upon by a field, the atoms of different elements respond in different ways; in particular, that the force arising from a particular concentration gradient in a binary alloy would cause the atoms of one component to move with a drift velocity which is in general different from that of the atoms of the other component. The recent experiments of Smigelskas and Kirkendall1 support this viewpoint, since they found, in essence, that during diffusion in alpha brass zinc moves appreciably faster than copper. This was evidenced by the relative motion of inert molybdenum wires. Such a phenomenon is incompatible with the place interchange theory of diffusion proposed by several authors, most recently by Birchenall and Mehl.2 This theory has, however, also been questioned3.4 for other reasons, principally because of the high energy required for direct atomic interchange. The rather large difference between self-diffusivity, as determined by tracer technique, and mutual diffusivity, as determined with the aid of another element at low concentration, might also be interpreted as favoring the above idea; however, Birchenall and Mehl have pointed out that there is another possible interpretation of this difference; this is discussed later. A rather interesting and pertinent observation was made by Schwartz,5 who noticed that tungsten lamp filaments, heated by direct current, commonly fail by necking down in the region at the temperature gradient near the positive end, with a concomitant swelling at the corresponding position near the negative end. He introduces considerable auxiliary evidence to show that this phenomenon is occasioned by the motion of tungsten cations which migrate in the high temperature region from the positive end toward the negative end. The mechanism of this migration is not clearly understood. If, however, this experimental evidence be accepted, we are forced to conclude that alloying elements in the tungsten may migrate by the same or a similar mechanism, whatever it may be, at a greater or lesser rate, thus giving rise

Jan 1, 1948

By C. Stansfield Hitchen

THE introduction of the logarithmic sector method of quantitative spectrography by Scheibe and Neuhäusser in 1928, and the subsequent .modification and improvement of the method by Twyman and Simeon, would seem to have marked yet a further advance in quantitative spec-trum analysis and its industrial application, inasmuch as it offers a simple means of eliminating some of the uncertainties inherent in the older methods based upon mere visual comparison of line intensities. In their recent admirable review of the position and capabilities of industrial spectroscopy, Brownsdon and van Someren1 say: Ways and means of facilitating the comparison of line-intensities so as to give them numerical values are helpful, and of these a logarithmic sector rotating in front of the slit appears to he one of the most promising; . . . the success recently experienced by the author in using this method for the examination of steels and solutions of metallic salts prompted him ,to investigate its possible use in estimating the impurities commonly present in crude and refined tin. The results of this investigation are submitted in the present paper. Details of a number of spectrographic analyses of tin for various impurities have already been published. Thus, Schweitzer2 describes the spectrographic examination of tin for lead, bismuth and cadmium, and was able to distinguish between such atomic percentages as 0.01, 0.05, 0.10, 0.30, 0.60, 1.20, 3.00 and 10.00. Negresco3 investigated the bismuth content of tin over a range of from 0.0005 to 35 per cent. Meggers, Kiess and Stimson4 compare spectrographic and chemical analyses of tin metal for copper, lead, iron, zinc, silver, nickel and bismuth. They stress also the value of spectrum analysis in the examination of tin used for boiler plugs, where the requirements that only minute quantities of impurities shall be present render the chemical analysis both tedious and difficult.

Jan 1, 1933

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 John H. Walthall, Raymond L. Copson, Travis P. Hignett

In October 1942, the War Production Board requested the Tennessee Valley Authority to undertake investigations to determine the feasibility of producing alumina suitable for reduction in aluminum cells, from clays and other domestic materials, by a lime-sintering, soda-ash leaching process. The work was undertaken by the chemical engineering staff of the Authority under the general direction of the War Metallurgy Committee of the National Academy of Sciences. The investigation included small-scale tests to determine the most suitable conditions for the process, and construction and operation of a pilot plant to obtain data for evaluation of the process and for design of a plant. The results of this investigation are described in the present paper. Sources of Alumina Alumina for the commercial production of aluminum is obtained from bauxite by the Bayer process. The tremendous demand for aluminum for wartime uses is causing rapid exhaustion of the high-grade bauxite deposits in the United States. On the other hand, there is an abundance of aluminous materials such as clay and lower grades of bauxite, which are not suitable for treatment by the Bayer process because of their high silica content. The Tennessee Valley Authority has conducted research and pilot-plant work for more than 5 years on methods for the production of alumina from clay and low-grade bauxite. Particular attention has been given to the high-grade white kaolin found in Carroll County, Tennessee. Exploratory drilling has demonstrated that at least 4 1/2 million tons of kaolin containing in excess of 34 per cent AlzOI is available in this area by strip-mining methods. It has been estimated that hundreds of millions of tons of clay of similar quality occur in the Tennessee Valley region. The Process The process is illustrated in the flowsheet (Fig. I), and consists essentially of the following steps: I. Heating a mixture of clay and limestone to form a sinter containing calcium aluminate and dicalcium silicate. z. Leaching this sinter with a dilute sodium carbonate solution, to form a sodium aluminate solution and a calcium carbonate, calcium silicate residue, which is discarded. 3. Treating the sodium aluminate solution with carbon dioxide to precipitate aluminum trihydrate and regenerate the sodium carbonate solution, which is recycled. 4. Heating the aluminum trihydrate to produce alumina. The process was considered promising because of the abundance and cheapness of the two raw materials, clay and limestone; and because, as compared with an acid process, smaller amounts of critical

Jan 1, 1944

By Shiro Ban-ya, John F. Elliott, John Chipman

The activity of carbon in Fe-C austenite at 1150°C has been determined for concentrations up to about 2.1 pct C using the equilibrium: C + COz = 2CO; equations have been derived expessing the activity as a function of carbon content on the basis of twelve mathematical models. Several of these represent the data satisfactorily. ACCURATE information on the thermodynamic properties of austenite in the binary system Fe-C is needed as a basis for studies of transformation and precipitation in steels of all sorts, alloy as well as plain carbon. The many attempts to approach this problem through statistical thermodynamics require sound and dependable experimental data in order to evaluate the several models which have been suggested. In this paper we are concerned with the experimental determination of the activity-composition relation in austenite at the temperature of its widest range of stability, approximately the eutectic temperature (1153°C). Accurate investigation of the activity of carbon in austenite may be said to have begun with the work of Dunwald and wagner.' A more detailed study was carried out by R. P. smith2 on the two equilibria: More recent work on these two equilibria has been reviewed by Chipman,3 who pointed out the experimental hazards associated with studies of Eq. [I]. Studies of this reaction involve rather small values of the ratio these are susceptible to errors due to traces of moisture in the apparatus according to the reaction: Ellis, Davidson, and Bodsworth4 evaluated K, for their experimental temperatures and used desiccants to control water vapor pressure. While they were able in this way to obtain consistent values for K1 it cannot be said that all of the uncertainties of the method have been overcome. Results by both methods reported by Schurmann, Schmidt, and wagener5 appear to be consistent except at very low carbon content. Reaction [2] was employed in the experimental work reported here. It is to be recognized, however, that it is not applicable to projected studies of certain alloy steel compositions involving stable oxide-formers.

Jan 1, 1970

By Ernst F. Eurich

Alexander Parkes patented in England in 1851-52-53 a process for desilvering lead by means of zinc, making use of the greater affinity of silver for zinc than for lead, discovered by Karsten in 1842. The efforts in England to develop it commercially were not particularly successful, nor was the attempted introduction into the United States. This last was not surprising, as it was about the beginning of our Civil War, and at that period there was very little lead-bullion produced in the United States and there was no field for the process here. There was at that time on Staten Island an establishment that pattisonized lead, probably from Rossie, N. Y., and Chester, Pa., and possibly some Spanish lead, but the production of lead-bullion in the Far West had not yet begun. In 1864, Edward Balbach, of Newark, N. J., patented in this country a process for desilvering lead by means of zinc, and in 1867 Edward Balbach, Jr., patented a " movable black-lead retort with a neck, placed in a furnace," for the purpose of distilling the alloy of zinc, lead, and the precious metals. A brief comparison of the Parkes and the Balbach processes is interesting. The Parkes process as practiced in England consisted in stirring into silver-bearing lead, melted in a kettle, from 1 to 2 per cent. of zinc, cooling, skimming the alloy of lead, zinc, and silver that rose to the surface, liquating it in an iron retort, distilling the residual rich alloy in fire-clay retorts, thus regaining the zinc, and refining the desilvered lead at a low heat in a shallow cast-iron pan that formed the hearth of a reverbera-tory furnace. If the lead was too impure, it was first softened

Jan 1, 1913

By W. J. Reagan

THE problem of increasing output and decreasing percentage of rejections is a vital one in the manufacture of steel of any kind. The making of basic open-hearth steel for use in rolled steel wheels, tires for locomotive and car wheels, and forgings of various kinds, is a highly specialized industry. The increase in weight of railway rolling stock of all kinds, and the high speed that the public demands of transportation facilities, make it imperative that steel for use in this class of material shall be of the highest quality obtainable. During the past few years it has been the writer's good fortune to have opportunity-to study the defects in basic open-hearth steel, and also the results obtained by various changes in open-hearth practice, on such defects. The opportunity for study and the details available are rarely found in the manufacture of steel of any kind. It seems reasonable to assume that many of the results determined here can be applied to the production of steel of other types with a decided improvement in quality, a decrease in the percentage of rejections and an increase in output. All of the material described is basic open-hearth steel with the following range of analysis: carbon, 0.50 to 0.85 per cent.; phosphorus and sulfur, 0.04 coax.; silicon, 0.15 to 0.35; manganese, 0.50 to 0.75. All of this material is bottom-cast, therefore tapping and pouring temperatures are higher than in top-cast production. Ingots used in this type of work are of standard length with varying diameters. The ingot is known as duodecagonal, or twelve-sided. The standard body length is 88 in. and the hot top length, 14 in. Fig. 1 shows a typical ingot of this type. The diameter varies from 13 to 30 in. Ingots for special forgings, which cannot be made in molds of standard size, are made in molds of various sizes and designs. These ingots are sliced cold, into blocks of various lengths, depending upon the weight of the forging to be made. Fig. 2 shows the ingot-after coming from the slicing lathe. Just sufficient metal remains between blocks to hold the ingot in one piece while it is being removed from the lathe; then steel wedges are inserted between the blocks and the blocks are broken apart. This affords abundant opportunity for inspection, as the interior of the

Jan 1, 1930

By C. A. Czako

INTRODUCTION In recent decades sintering and pelletizing of finely divided materials have become the primary tonnage producing modes of agglomeration. This statement is especially true in the iron and steel industry and, to a lesser degree, in the nonferrous, chemical and non-metallic minerals processing industries. In every industry the main objectives in agglomerating fines are essentially the same, namely to convert ores, minerals and chemicals of undesirable fineness into agglomerates characterized by a size consistency desirable for subsequent use or processing. Depending on the type of agglomeration process selected and the conditions maintained during agglomeration, the physical process of increasing size is complemented by a number of other unit processes. These processes can occur simultaneously, consecutively or in an overlapping manner. Some of these additional unit processes are incidental to the agglomeration operation, but at the same time can be critical, depending upon the subsequent use of the product. Accordingly, during processing, conditions have to be controlled to either suppress or enhance the extent of completion of these unit processes. The purpose of this report is to review laboratory testing as the basis for engineering modern sintering and pelletizing plants. Considering that most typical applications are for the iron and steel industry, agglomeration of ferrous materials is reviewed and discussed. When these total processes are adapted to suit non- ferrous materials, chemicals, or non-metallic substances, the over- all approach remains the same; only the processing parameters are affected as necessitated by the different nature of the materials.

Jan 1, 1977