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By L. W. Kempf, K. R. Van Horn

Plastic deformation of most commercia1 metals within a sufficiently low temperature range results in profound changes in structure and properties, of which the causes and effects are not completely understood. One of these effects is the presence of internal residual stresses and strains, which ordinarily do not appear to require specific consideration in most structural applications but which may be quite undesirable in particular instances. For example, in heavy sections that require considerable machining before assembly, residual stresses may be undesirable because of the distortion they cause when their balance is disturbed by machining or otherwise. In addition, the distribution of stresses may be such that it acts in the same direction as the applied load, thus bringing about premature failure or reducing the load-carrying capacity of the member. One source of residual stress in metal structures is the plastic deformation that may occur during rapid cooling from relatively elevated temperatures, as in the cooling of a casting in the mold or the quenching of a heavy section from elevated temperatures during heat-treatment. These residual stresses are usually undesirable because their direction of operation and magnitude cannot be controlled well enough to permit utilization of the changes in properties of the metal that they may bring about. The most convenient manner of controlling such residual stress is by proper selection of the cooling rate or by reheating to a temperature at which plastic flow can take place, resulting in relief of the residual stresses and strains. Both of these methods of control, however, may cause a reduction in the optimum properties obtainable from the previous operation. A compromise must be struck, and if it is to result in the best possible combinations of properties, specific information must be available regarding the magnitude of the stresses and the rate at which they are affected by variations in cooling rate or in reheating temperature. The complete quantitative estimation of residual stress in complicated metal shapes is exceedingly difficult, if not impossible. In simple sections, however, relatively quantitative analysis may be applied and useful cstimations of stress distribution may be made. This paper is concerned largely with the rate of relief, upon reheating, of internal residual stress in simple aluminum-alloy structures. Since even with simple structures quantitative estimation of residual stresses is laborious and costly, an attempt was made to find other means of collecting data upon which commercial heat-treatments might be based. Incidentally, a few data were collected bearing on the problem of relaxation of aluminum alloys. Determination of Residual Stresses The magnitude and distribution of residual stresses in simple aluminum-alloy shapes rapidly cooled from elevated temperatures has been discussed in a previous paper.' Fig. I reproduces some of the data

Jan 1, 1942

By William A. Johnson

THE mathematical analysis of diffusion curves in solid metals is Carried out ordinarily by analogy with the flow of heat in a continuous medium and no account is taken of the fact that the materials involved are composed of discrete particles that move discrete distances at irregular intervals. It is possible to treat the problem on the basis of simple assumed atomic mechanisms, in which case, because of the small scale of the elementary process compared to the gross effects observed experimentally, the two procedures lead to the same expression for the variation of concentration with distance. Thus, for engineering purposes, the usual methods are quite satisfactory. If, on the other hand, our purpose is to go beyond the mere collection of data, however desirable this may be, it is necessary to recognize and understand the factors that are of fundamental importance. One factor that has not hitherto been considered when dealing with solid metals is the difference in atomic weights of the isotopes of a single metal. While all the atoms of a given element are alike chemically, their weights may vary by a small but significant amount, and atoms of different weights may have different diffusion rates. With gases this variation in isotopic weight produces a change in the rate of diffusion by a factor inversely proportional to the square root of mass. While, except for the lightest gases, this is not a large effect, it is, for example, sufficient to permit a considerable concentration of one isotope at the expense of others. If metals exhibit a similar phenomenon, some modification of the analysis of the diffusion process will be required, since the different isotopes of a given metal will have different probabilities of moving and the heat-flow analogy will contain a fundamental error. This situation cannot be rectified by using a diffusion coefficient based on the average probability of moving, and it can be shown that even when the diffusion coefficient is independent of composition, the diffusion curve will not agree with the simple theory except in the rare cases where only one isotope exists; e.g., gold. If, however, the mass effect in the solid state were no larger than in the gaseous, the errors arising therefrom in the analysis of ordinary diffusion curves would be quite negligible. Nevertheless, our desire to obtain all possible information concerning the details of the diffusion process, and the possibility of diffusion in the solid state as a means for separating isotopes are cogent reasons for undertaking an experimental study to determine whether isotopes of different masses diffuse at different rates. EXPERIMENTAL PROCEDURE If isotopes of different masses diffuse at different rates, the ratio of the concentration of one relative to another will vary with the distance from the diffusion inter-

Jan 1, 1946

By E. W. Davis

If the tonnage of merchantable iron ore remaining in the Lake Superior district is divided by the average of the annual shipments for the past 20 years, it will be found that this ore supply will be exhausted in approximately 35 years. This computed exhaustion period would be an indication of the future activities of the iron-mining industry if it were not for the fact that merchantable ore is being manufactured from low-grade ore, of which there is an almost inexhaustible supply in the Lake Superior district. It is true that at present only the simplest of these low-grade ores are being concentrated to any considerable extent, but progress is being made with the treatment of the more complex ores, and now, in addition to 20 washing plants on the Mesabi Range, three plants are equipped with jigs for the treatment of ore that cannot be concentrated simply by washing. The latest addition to the ore-treating plants of the Mesabi Range is a magnetic roasting and concentration plant at Cooley, Minn., in which ore that cannot be concentrated either by washing or by jigging is roasted to the magnetic state and concentrated on magnetic separators. This plant is beginning its third season of operation, and while it is too soon to make definite predictions, there are strong indications that this new process may make commercially possible the manufacture of high-grade, merchantable iron ore from large quantities of low-grade ore now considered worthless. After the iron oxide contained in an ore has been converted to magnetite, almost any desired grade of concentrate can be produced, using magnetic-concentration equipment of the types now in general use for the concentration of the natural magnetites of New York, New Jersey and Pennsylvania. The conversion of hematite (Fe203) to magnetite (Fe3O4) is easily accomplished by heating the ore to a dull red temperature in a reducing atmosphere. The reaction is slightly endothermic, and while it requires 200 B.t.u. to heat to 900' F. one pound of hematite ore containing 45 per cent Fe, it requires only 100 B.t.u. to convert the oxide into magnetite. In the laboratory, using small quantities of ore, this conversion is very simple, but large furnaces suitable for commercial

Jan 1, 1939

By E. W. Davis

IF the tonnage of merchantable iron ore remaining in the Lake Superior district is divided by the average of the annual shipments for the past 20 years, it will be found that this ore supply will be exhausted in approximately 35 years. This computed exhaustion period would be an indication of the future activities of the iron-mining industry if it were not for the fact that merchantable ore is being manufactured from low-grade ore, of which there is an almost inexhaustible supply in the Lake Superior district. It is true that at present only the simplest of these low-grade ores are being concentrated to any considerable extent, but progress is being made with the treatment of the more complex ores, and now, in addition to 20 washing plants on the Mesabi Range, three plants are equipped with jigs for the treatment of ore that cannot be concentrated simply by washing. The latest addition to the ore-treating plants of the Mesabi Range is a magnetic roasting and concentration plant at Cooley, Minn., in which ore that cannot be concentrated either by washing or by jigging is roasted to the magnetic state and concentrated on magnetic separators. This plant is beginning its third season of operation, and while it is too soon to make definite predictions, there are strong indica-tions that this new process may make commercially possible the manu-facture of high-grade, merchantable iron ore from large quantities of low-grade ore now considered worthless. After the iron oxide contained in an ore has been converted to mag-netite, almost any desired grade of concentrate can be produced, using magnetic-concentration equipment of the types now in general use for the concentration of the natural magnetites of New York, New Jersey and Pennsylvania. The conversion of hematite (Fe203) to magnetite (Fe304) is easily accomplished by heating the ore to a dull red tempera-ture in a reducing atmosphere. The reaction is slightly endothermic, and while it requires 200 B.t.u. to heat to 900° F. one pound of hematite ore containing 45 per cent Fe, it requires only 100 B.t.u. to convert the oxide into magnetite. In the laboratory, using small quantities of ore, this conversion is very simple, but large furnaces suitable for commercial

Jan 1, 1936

By Roman Šejnoha, Karel Mazanec

A pronounced tendency for delayed fracture zoas observed in the martensite structure of low-alloy steels in the as-quenched condition. Cracks of predominantly intercrystalline nature nucleated and propagated at stresses substantially lower than the short-titne tensile strength of- the steels, and were observed even in hydrogen-free speciunens. The occurrence of delayed fractures in the as-quenched condition is interpreted as a supevposition of the effect of free dislocations generated during the martensite transforlnation, and of a weakening of the prior austenite grain boundaries caused by dynamic shocks exerted on the boundaries by growing martensite plates. AN important metallurgical problem, connected with the production and use of high-strength steels, is delayed fracture in martensitic structures. Such fractures occur in quenched steels as a result of prolonged loading with external stresses far lower than the short-time tensile strength of the steel. The same effect can be produced by sufficiently high internal stresses: it is well-known that quenched structures will in some cases crack intergranularly at room temperature if not tempered quickly enough even in the absence of any externally applied stress. In Troiano's papers1,2 on delayed fractures in high-strength steels, the fundamental role of hydrogen migrating under the influence of multiaxial stress towards the nuclei of cracks was found. Fig. 1 shows the typical relationship between stress and the time to fracture found by Troiano in hydrogen-charged high-strength steels. On the other hand, Shurakov 3,4 explains the realization of delayed fractures in martensite as due to a "quasi-viscous" behavior of the austenite grain boundaries immediately after the martensitic transformation. 1) MATERIALS AND EXPERIMENTAL METHODS Two low-alloy steels of commercial purity were used for the experiments reported in this paper. Their chemical composition is shown in Table I. The heats were melted in a laboratory furnace, cast to ingots, forged to bars of 3/4 in. diameter, and annealed. Machined test pieces were heat-treated as follows: Ni-Cr-Mo steel held at 900°C for 30 min and quenched in oil; Mn-Si-Cr steel held at 900°C for 30 min and quenched in water. For the delayed-fracture tests, notched cylindrical test pieces, Fig. 2, stressed in torsion, and unnotched cylindrical tensile-test pieces, 1/4 in. diameter, were used. The specimens were normally loaded with a constant static load 45 min after quenching for the torsional tests and 10 min

Jan 1, 1965

By John Chipman

IN the manufacture of rimming steel-which constitutes the bulk of the world's production of mild steel-the factors that determine the quality of the product are very closely associated with the pouring and solidification of the steel in the ingot mold. The behavior of the metal in the mold is, on the one hand, the resultant of the complex processes through which the liquid metal has passed, and, on the other, it is an indication of the probable behavior of the ingot during subsequent rolling and finishing operations. A detailed study of the mechanism of solidifica-tion of rimming ingots ought to yield information that will be useful iii controlling the structure of the ingot and the quality of the ultimate product. The first step in such a study is to determine the rate at which the solid shell of the ingot forms from the liquid metal in the mold. A knowledge of the rate of solidification will make it possible to correlate observations of rimming action and gas evolution with studies of the structure, porosity, and segregation within the ingot. Thus, if the metal in the mold is observed to fall, let us say one minute after pouring, the portion of the structure associated with this fall will lie located in the part of the ingot that is solidifying at that particular moment. The knowledge that the ingot solidifies to a depth of ¾ in. in the first minute enables us to locate in the ingot the structural features corresponding to the observed fall. Conversely, the blowhole condition associated with a rising or growing ingot will be found in the part of the ingot that is solidifying at the time the phenomenon occurs. The time required for the complete solidification of an ingot has long been a matter of speculation. It is of considerable practical importance in connection with charging and heating in the soaking pits. Too rapid handling of the ingot through heating and rolling processes has been thought to be associated-with excessive pipe and other internal defects, so that a further object of this investigation was to attempt to estimate the time required for complete solidification, or the minimum practical time within which the subsequent operations can be performed with the minimum hazard.

Jan 1, 1937

By E. W. Davis

If the tonnage of merchantable iron ore remaining in the Lake Superior district is divided by the average of the annual shipments for the past 20 years, it will be found that this ore supply will be exhausted in approximately 35 years. This computed exhaustion period would be an indication of the future activities of the iron-mining industry if it were not for the fact that merchantable ore is being manufactured from low-grade ore, of which there is an almost inexhaustible supply in the Lake Superior district. It is true that at present only the simplest of these low-grade ores are being concentrated to any considerable extent, but progress is being made with the treatment of the more complex ores, and now, in addition to 20 washing plants on the Mesabi Range, three plants are equipped with jigs for the treatment of ore that cannot be concentrated simply by washing. The latest addition to the ore-treating plants of the Mesabi Range is a magnetic roasting and concentration plant at Cooley, Minn., in which ore that cannot be concentrated either by washing or by jigging is roasted to the magnetic state and concentrated on magnetic separators. This plant is beginning its third season of operation, and while it is too soon to make definite predictions, there are strong indications that this new process may make commercially possible the manufacture of high-grade, merchantable iron ore from large quantities of low-grade ore now considered worthless. After the iron oxide contained in an ore has been converted to magnetite, almost any desired grade of concentrate can be produced, using magnetic-concentration equipment of the types now in general use for the concentration of the natural magnetites of New York, New Jersey and Pennsylvania. The conversion of hematite (Fe203) to magnetite (Fe3O4) is easily accomplished by heating the ore to a dull red temperature in a reducing atmosphere. The reaction is slightly endothermic, and while it requires 200 B.t.u. to heat to 900' F. one pound of hematite ore containing 45 per cent Fe, it requires only 100 B.t.u. to convert the oxide into magnetite. In the laboratory, using small quantities of ore, this conversion is very simple, but large furnaces suitable for commercial

Jan 1, 1939

By C. L. Mantell

ALTHOUGH SO common and well known a metal, tin is really a less abundant element than many of those less familiar and usually ranked with the scarce or rare elements, such as cerium, yttrium, lithium, beryllium., titanium, zirconium and vanadium. The color of tin is white, with a slightly bluish tinge. When it is compared with nickel, the latter metal is brown. When placed alongside of tin, chromium is definitely blue. Tin is whiter than silver or zinc. Exceedingly thin films of tin show various shades of brown by transmitted light. The metal has a brilliant luster, and when mirror-polished, has high light reflectivity. The luster depends to a large extent upon the pouring temperature at which the metal is cast. If the temperature be, too high, iridescent colors may show on the surface. These are the result of oxide film formation. If the pouring temperature be too low, the surface is dull. Small amounts of foreign metals, such as lead, arsenic, antimony and iron, decrease the luster of tin and impart a yellowish tinge to the metal. The structure is decidedly crystalline. The cast metal is a mass of crystals. When a bar of tin is bent, it emits a characteristic creaking sound. This is called the "cry" of tin, resulting from the grinding of the crystals one against the other during the bending of the metal. Tin metal may lose its crystalline structure by cold working, but grain growth occurs rapidly under the influence of heat. Metal which has been cast at a low temperature may become amorphous as the result of mechanical work. If such material be heated to temperatures well. below the melting point, say at 110° C. for a half hour or for a few minutes at 150° C. recrystallization occurs. If the surface of tinned plate, tin foil, or tin metal in cast form be etched with hydrochloric acid containing a little free chlorine, attack occurs at the intercrystalline faces. The surface shows patterns resembling the frost flowers on window panes in winter. The etched appearance is called moiré metallique. Fine dendritic surface crystals of tin may be obtained by casting the metal on a surface of polished steel. In commercial tin plate, the intercrystalline boundaries are shown by fine grooves or channels, which result from the method

Jan 1, 1929

By Alexander Squire

A brief study of the effects of material and processing variations upon the tensile properties of steel formed from mixtures of iron and carbon was made in order to provide information regarding the properties obtainable in iron-carbon compacts as influenced by forming pressure, sintering temperature, and graphite particle size. Sintered steels formed from mixtures of iron and graphite have been studied by Stern,' who investigated the effect of various percentages of graphite on compacts formed from electrolytic iron that were repressed and heat-treated after sintering. A further study, by Stern and Greenberg,l is concerned with the heat-treatment of steels formed by the car-burization of iron compacts, and Margolies3 has reported work on the simultaneous sintering and carburization of iron-powder parts. Glauch4 investigated the effect of various types of graphite on the properties of iron-carbon powder alloys but did not determine the effect of different particle sizes of the same graphite alloyed with different types of powder. In the investigation reported in this paper, powders typical of those produced by electrolytic deposition and the decar-burization of shotted steel scrap were used. The powders were mixed by tumbling in a jar mill with graphite powder ground to an average particle diameter of 2, 4, 6, and 16 microns (as determined by microscopic measurement). The properties of the iron and graphite powders are presented in tabular form as Table I. In order to obtain the maximum information from a minimum number of test specimens, the study was divided into two sections with one set of specimens treated identically in each section as a basis for comparison. In the first section, iron powder produced by the shotting and subsequent decarburization of scrap steel was mixed with 2-micron graphite powder, pressed at 50,000, 100,-000, and 200,000 psi, and sintered in hydrogen at 1200°C for the periods of time ranging from 15 to 120 minutes. In the second section of the investigation, electrolytic iron powder was mixed with graphite of an average particle diameter of 2, 4, 6, and 16 microns, pressed at 100,000 psi, and sintered at temperatures ranging from 1000° to r200°C'. for periods of time of 30 to 180 minutes. By following this procedure an indication of the effect of the following variables upon the density and tensile properties of iron-carbon powder compacts was obtained: (I) forming pressure, (2) sintering time, (3) particle size of graphite powder, (4) sintering temperature, (4) type of iron powder.

Jan 1, 1947

By Alexander Squire

A brief study of the effects of material and processing variations upon the tensile properties of steel formed from mixtures of iron and carbon was made in order to provide information regarding the properties obtainable in iron-carbon compacts as influenced by forming pressure, sintering temperature, and graphite particle size. Sintered steels formed from mixtures of iron and graphite have been studied by Stern,' who investigated the effect of various percentages of graphite on compacts formed from electrolytic iron that were repressed and heat-treated after sintering. A further study, by Stern and Greenberg,l is concerned with the heat-treatment of steels formed by the car-burization of iron compacts, and Margolies3 has reported work on the simultaneous sintering and carburization of iron-powder parts. Glauch4 investigated the effect of various types of graphite on the properties of iron-carbon powder alloys but did not determine the effect of different particle sizes of the same graphite alloyed with different types of powder. In the investigation reported in this paper, powders typical of those produced by electrolytic deposition and the decar-burization of shotted steel scrap were used. The powders were mixed by tumbling in a jar mill with graphite powder ground to an average particle diameter of 2, 4, 6, and 16 microns (as determined by microscopic measurement). The properties of the iron and graphite powders are presented in tabular form as Table I. In order to obtain the maximum information from a minimum number of test specimens, the study was divided into two sections with one set of specimens treated identically in each section as a basis for comparison. In the first section, iron powder produced by the shotting and subsequent decarburization of scrap steel was mixed with 2-micron graphite powder, pressed at 50,000, 100,-000, and 200,000 psi, and sintered in hydrogen at 1200°C for the periods of time ranging from 15 to 120 minutes. In the second section of the investigation, electrolytic iron powder was mixed with graphite of an average particle diameter of 2, 4, 6, and 16 microns, pressed at 100,000 psi, and sintered at temperatures ranging from 1000° to r200°C'. for periods of time of 30 to 180 minutes. By following this procedure an indication of the effect of the following variables upon the density and tensile properties of iron-carbon powder compacts was obtained: (I) forming pressure, (2) sintering time, (3) particle size of graphite powder, (4) sintering temperature, (4) type of iron powder.

Jan 1, 1947

By R. S. Dean

BLUE HEAT PHENOMENA IN constructing a theory of the flow and hardening of metals, we necessarily make use of such phenomena as seem to be, universally observed in metals. It is, therefore, a matter of. concern to the constructors of such mnemonic systems if one or two of the group classified as metals show anomalous behavior. Such egregious phenomena are observed in pure or nearly-pure iron in the reaction of its mechanical properties to low-temperature annealing after cold work and to increased temperature of testing. In short it has been generally observed that iron," as an outstanding exception among metals, increases its hardness and strength by low-temperature annealing. after cold work,1 and also by increase of testing temperature to the range of 150° to 300° C. The investigation here recorded was made then with the object of ascertaining if similar phenomena were observed in high purity iron and, if not, to the presence of which impurities these phenomena could be traced.

Jan 1, 1929

By L. W. Swent

Dr. Emrick, honored guests, distinguished speakers, ladies and gentlemen, I am Langan Swent, Vice President for Environmental Affairs and Occupational Safety and Health, of Homestake Mining Company. Today, I appear on behalf of the American Mining Congress, as chairman of its uranium mine health subcommittee. The American Mining Congress is a trade association of several hundred members, which include the producers of a large proportion of the nation's uranium. I've been asked to make a statement of principles for the uranium industry. There are two types of principles that apply to industry in general, and specifically to the uranium industry. Some have external origins and apply regardless of what industry does or thinks. Others are generated by industry itself and serve as goals for the industry. I'll discuss some of each type. I'll limit my statement to those principles related to the subject of this conference--radiation hazards in mining. I won't take your time trying to explain some of the unrelated principles that we must all contend with, such as Parkinson's Laws, Murphy's Law, and the Peter Principle. First and foremost, industry has a sincere interest in the well-being and health of its employees. There are two basic reasons for this. One is a basic respect for human lives, especially those of people we see and work with every day. No one in management wants to carry the lifelong burden of blame for a life lost due to poor working conditions. Most uranium and other mining is done in small communities. Production workers, maintenance workers, service workers, shift bosses, foremen, superintendents and managers all live in the same community. They attend the same churches. They serve together in civic activities. Their children go to the same schools. If one employee in such a community loses his life due to poor working conditions, those remaining know in a daily and intimate way the resulting personal tragedy, usually of a bereaved widow and fatherless children. This sad experience makes the community, including industry management, intensely sensitive to the need for maintaining good working conditions in the mines. But what about the segment of industry that does not live in the mining communities? Corporate and owner's offices are frequently hundreds of miles from the communities where the mining takes place. Many of these people are not personally acquainted with the workers, and there are few close personal ties between the two communities. The distant staff are, however, still human beings and motivated by the same basic human respect for life. Mr. Manuel Gomez of MSHA and a member of the planning committee for this conference summed this point up expressively when he told me: "No one group has a corner on compassion." In addition to compassion, there is another factor. In both communities the basic assignment to everyone is to produce profits. In carrying out this assignment, supervisory and management people are acutely aware of the high cost of illnesses and accidents. Their objective of maximizing profits is advanced significantly by minimizing illnesses and accidents at the mines. A business that has illnesses and accidents generally suffers from poor employee morale and high employee turnover, both of which detract from profits. Next, I would like to talk about what industry has done in the field that is the subject of this conference. We have worked at all sorts of methods to reduce exposure of employees since the exposure standards were first introduced and then lowered. Other speakers will go into details of technology, and I'll simply comment on exposure results. These are best shown in Table 1. The table shows the average WL to which miners in U.S. underground uranium mines have been exposed since 1937 through 1980. The trend of decreasing radon daughter concentrations throughout the period is obvious. Figure 1 presents this data graphically and shows the trend at a glance. This record begins in 1937 when uranium, as such, really wasn't being mined or sought. The concentrations given by the U.S. Public Health Service were for a few small vanadium mines which carried uranium as a by-product. A few years later, when the Manhattan project to develop the atomic bomb was begun, these mines became the first U.S. uranium mines and the vanadium became the by-product! The radiation hazard then also received attention and the average concentrations began to decline. As knowledge of the reality of the hazard spread, conditions improved. The search for uranium in the U.S. turned up new and larger ore bodies that had to be mined by large underground mines. These mines involved ventilation planning from the beginning, and when they came into production in the late 1950's they lowered the average concentrations greatly. Then in 1960 the American Standards Association adopted a standard setting 1 working level as a satisfactory condition, and several action levels up to 10WL, at which point removal of people from exposure was called for. As a result of the uranium producing states governors' conference in December 1960, state mine inspection agencies, in the early 1960's, began to adopt and enforce the ASA standards. As a result, average concentrations again declined. In 1967, the Federal Radiation Council recommended an annual limitation of 12 WLM per individual. This represented a great change in the methods of

Jan 1, 1981

By P. J. A. Beukes, C. C. La Grange

INTRODUCTION Some years ago the authors proposed a modified procedure1 for carrying out micum index determinations2. The modifications consisted of using a drum of 50 cm internal length, i.e. half the length of the standard micum drum (a modification also adopted by the B.S.J.3), and the use of a + 25 mm coke instead of + 60 mm coke for the test. The proposed modified test and formulae for converting results obtained from it to standard micum test results and vice versa were based on the results obtained during the investigation of about 200 test cokes made in ovens of the South African Steel Industrial Corporation Limited (Iscor), the Fuel Research Institute co-operating with the experiments. Extensive testing of cokes has since been done at the Fuel Research Institute using both the standard and the modified procedures. The numerous test results obtained during this trial period fully support and strengthen the confidence originally expressed by the authors in the modified testing procedure. The scope of the modified micum index determination has in the meantime been extended by applying the testing procedure also to test cokes made in the Institute's experimental coke ovens, and also in this case the modified procedure has proved its usefulness. A difficulty is that when comparing the characteristics of cokes made in the Institute's two experimental coke ovens with each other and with those of cokes made from similar blends in commercial coke ovens, for example those of Iscor, the index values obtained invariably do not check exactly due mainly to inherent differences between the different types of oven4. For instance, resistance to abrasion of a coke made in Iscor's ovens is always appreciably higher than that of a coke made from the same blend (and having a similar moisture content) in the experimental ovens. This makes direct comparisons and the prediction of quality to be expected from commercial products, based on experimental coke oven results, difficult. It may also be added that workers in Great Britain some years ago reported a similar experience5. In the authors' opinion the main reason for the discrepancy is the relatively low height of the experimental ovens resulting in a much lower static pressure on the charge during coking than that obtaining in a commercial oven. The difficulty was pointed out and briefly discussed in a publication4 which appeared at a time when the micum test for coke evaluation had only just been introduced at the Institute, so that only B.S. shatter and abrasion test results were available for discussion in the publication. Needless to say, the introduction of the micum test by no means solved nor even alleviated the problem. On numerous occasions during the past few years the Institute has had to conduct contract investigations in its experimental coke ovens on behalf of companies which invariably desired an indication of the quality of coke likely to be obtained from certain coals or blends when coked commercially, more particularly in Iscor's type of coke ovens. It was, therefore, essential to accumulate statistical data which would enabe the prediction to be readily made. Fortunately the compilation of comparative coke-quality index values for the three types of oven under consideration has become possible as a result of coking investigations conducted in co-operation with Iscor over a number of years. During this period Iscor, on numerous occasions, kindly made available to the Institute portions of coals and blends coked in the Corporation's coke ovens, thus enabling parallel coking tests to be carried out in the Institute's experimental ovens. In this way enough statistical data became available to establish relationships between coking results obtained in Iscor's ovens and results obtained on similar coal charges in the Institute's ovens. The most practical and acceptable method of overcoming the problems of finding a suitable and simple basis enabling direct comparison between the cokes of the different origins mentioned to be made, is the assignment of descriptive arbitrary quality ratings, as indicated below, to the cokes obtained, it being argued that the quality rating assigned to coke made from a given coal or blend in the different coke ovens under standardized conditions should be the same, irrespective of differences in the index values obtained when subjecting the cokes to the usual coke evaluation tests. The system, which should enable the sponsors of coking investigations in the Institute's experimental ovens to make their own interpretations of the results obtained, is explained below. ARBITRARY QUALITY CLASSIFICATION OF COKES The Ml0m index1 (percentage material smaller than 10 mm after the test) of a blast furnace coke is a measure of its tendency towards breeze formation during handling -a low value indicating a low tendency. This is generally of greater importance under ruling South African conditions, than the M'40 index1 (percentage material larger than 40 mm after the test), which can be regarded as a measure of resistance to shatter. In fact, if the M10m value of a coke as made in Iscor's ovens is higher than about 11, the tendency of the coke to form breeze during handling and in the blast furnace is relatively so high that hardly any notice need be taken of its M'40 value, even if this is comparatively high. For this reason, therefore, much more weight should normally be assigned to Ml0m indices in the quality evaluation of cokes made from South African coking coals and blends, as the coals

By P. A. Laxen, H. R. Spedden, A. M. Gaudin

WHEN a mineral particle is fractured, bonds between the atoms are broken. The unsatisfied forces that appear at the newly formed surface1 are considered to be responsible for the adsorption of ions at the mineral surface. A knowledge of the mechanism and extent of ion sorption from solution onto a mineral surface is of interest in the development of the theory of flotation.2,3 Study of the adsorption of sodium from an aqueous solution on quartz offers a simple approach to this complicated problem. The availability of a radioisotope as a tracer element meant that accurate data could be obtained.4,5 Three main factors which appeared likely to affect the adsorption of sodium are: 1-concentration of sodium in the solution, 2-concentration of other cations in the solution, and 3-anions present in the solution. Hydrogen and hydroxyl ions are always present in an aqueous solution. By controlling the pH, the concentration of these two ions was kept constant. The variation in the amount of sodium adsorbed with variation in sodium concentration was then determined under conditions standardized in regard to hydrogen ion. The effect of concentration of hydrogen ions and of other cations was also measured. A few experiments were made to get a preliminary idea on the effect of anions. The active isotope of sodium was available as sodium nitrate. Standard sodium nitrate solutions were used throughout these experiments except when the effects of other anions were studied. It was found that sodium adsorption increased with sodium-ion concentration, but less rapidly than in proportion to it. Increasing hydrogen-ion concentration, or conversely decreasing hydroxylion, brings about a comparatively slight decrease in sodium-ion adsorption. Increasing the concentration of cations other than hydrogen or sodium decreases somewhat the adsorption of sodium ion. It would appear as if the kind of anion is a secondary factor in guiding the amount of sodium ion that is adsorbed. Materials and Methods Quartz The quartz was prepared as in previous work in the Robert H. Richards Mineral Engineering Laboratory4 except for the refinement of using de-ionized distilled water for the final washing of the sized quartz, prior to drying5 To minimize the laborious preparation of quartz, experiments were made to determine whether the sodium-covered quartz could be washed free of sodium and re-used. The experiments were successful as indicated by lack of Na' activity on the repurified material and by its characteristic sodium adsorption. Table I gives the spectrographic analyses of the quartz used. The quartz ranged from 16 to 40 microns in size, averaging about 23 microns (microscope measurement), and had a surface of 1850 sq cm per g (lot I), 2210 (lot II) and 2000 (lot III) as determined by the Bloecher method.6 Radioactive Sodium Method of Beta Counting for Adsorbed Sodium: Na22, the radioisotope of sodium, possesses convenient properties.7 It has a half-life of 3 years, thus requiring no allowance for decay during an experiment. On decay it emits a 0.575 mev ß radiation and a 1.30 mev ? radiation. The decay scheme is illustrated in the following equation: [Y Nam S. - 'Net 3 years] The ß radiation is sufficiently strong to penetrate an end-window type of Geiger-Mueller counting tube. This, in turn, makes it possible to use external counting, a great advantage in technique. Furthermore, it permits the assaying of solids arranged in infinite thickness, while assaying evaporated liquors on standardized planchets. The equipment used was standard and similar to that employed by Chang8 The original active material was 1 ml of solution containing 1 millicurie of Na22 as nitrate. This active solution was diluted to 1000 ml. Five milliliters of this diluted active solution was found to give a quartz sample a sufficiently high activity for accurate evaluation of the sodium partition in the adsorption measurements. Also, 1 ml of final solution gave a sufficiently high count for precision on the liquor analyses. The sodium concentration of the diluted active solution was 1.2 mg per liter, so that 6 mg of sodium for 60 ml of test solution and 12 g of quartz was the minimum amount used. The active solution was stored in a Saftepak bottle. Procedure for Adsorption Tests: The method consisted of agitating 12 g of quartz with 60 ml of solution of known sodium concentration for enough time to establish equilibrium between the solution and the quartz surface. The quartz was separated as completely as possible from the solution by filtering and centrifuging. The activity on the quartz and in the equilibrium solution was measured and the partition of the sodium was calculated from the resulting data. The detailed procedure for the adsorption test is set forth in a thesis by Laxen5 In brief, it included the following steps: 1-Ascertainment of linearity between concentration of Na22 and activity measured. 2-Evaluation of factor to translate activity on solid of infinite thickness in terms of activity on an evaporated active film of minute thickness, on the various shelves of the counter shield. 3-Taking precautions to avoid evaporation of water during centrifuging.

Jan 1, 1952

By M. Cross, K. Pericleous, A. Mouchmov

"Copper - nickel - sulphide alloys are typically cooled and solidified in 4, 8 and 16 tonne ingots. These ingots exhibit a variation of grain size distribution and macro segregation of the prime alloy components throughout. The former is assumed to be primarily due to the dominant relation between grain growth rate and the cooling profile, whilst the latter is heavily influenced by buoyancy driven residual convection. The objective of this research program is to examine the extent to which it is possible to develop a 'broad brush' computational model of this ingot cooling process, that can predict some 'integral' measure of the grain size (e.g. average diameter) and the macro-segregation as a function of operating conditions.A computational modeling software framework, PHYSICA+ is used to simulate the complex process of ingot casting, which involves coupling between different physical phenomena. The entire model involves:(i) a 'broad brush' grain growth model that could be used in the prediction of micro/macro-structure of alloy ingot cooling processes,(ii) a heat transfer and solidification model which takes into account a second phase transformation of P NhS2 to heazlewoodite, and (iii) NS fluid flow simulation which provides a good basis for further micro/macro segregation modeling.At this stage some results of the 3D convection driven thermal cooling and solidification profiles will be shown, together with the 'integral' model for the grain size prediction."

Jan 1, 2001

By R. A. Stauffer

The chief ore of lithium is spodumene, a lithium-aluminum silicate containing up to 3 pct lithium. The preparation of lithium salts from spodumene is costly because of the low concentration of the metal and the difficulty of separating it from the other alkali metals present. Dr. Kroll's and Dr. Schlecten's recent paper1 has reviewed various methods proposed for preparation of lithium. It will be seen from this paper that the methods proposed to date have required one or another of the lithium salts as a raw material. The high cost of these salts has been the chief item of expense in the lithium metal produced. This situation has made it interesting to investigate the possibility of producing the metal directly from spodumene. When spodumene is calcined at 1000ºC in the presence of lime, lithium oxide is replaced in the ore as is evidenced by the fact that it may be leached from the reaction mixture with water.2 Free energy calculations suggested that lithium oxide might be reduced with aluminum or silicon and the lithium produced distilled from the reaction mixture by heating-to about 1000ºC in a vacuum. These facts taken together suggested that it might be possible to prepare lithium metal directly from spodumene by heating a mixture of the ore, lime, and a suitable reducing agent in vacuum and distilling off the lithium metal as formed. The Replacement of Li2O in Spodumene A series of experiments were undertaken to determine the ratio of lime to spodumene necessary to free substantially all the lithium oxide Present in the Ore. The spodumene used in these experiments was supplied by Foote Mineral Co. in the form of powder of about 200 mesh' Analysis of the spodumene was as follows: PCT SiO2......................... 62.7 Al2O3........................ 29.9 Li2o......................... 4.9 Na2O........................ 0.89 CaO......................... 0.75 MgO........................ 0.49 K2O......................... 0.44 Lime (cp —200 mesh) was added in various ratios to spodumene and thoroughly mixed in a ball mill. Two hundred gram samples of spodumene-lime mixtures were charged loosely in fireclay crucibles and held at 1000ºC in a gas-fired furnace for 5 hrs. The product in each case was ground to pass 140 mesh and then placed in a thimble in a soxhlet extractor. Extraction with water was carried on for 6 hrs. After this period the extract was reduced in volume by evaporation in order to precipitate dissolved lime and was then filtered and titrated with 1/4 normal hydrochloric acid. After correcting for residual calcium oxide in solution, the alkali present was calculated as lithium oxide. The results of these experiments are shown in Table I and Fig I. At lime-spodumene ratios less than 1.5, the products were invariably fused. At the ratio of 1.5 and above, the product was loosely sintered with little evidence of fusion. When the ratio of lime to spodumene was three, replacement of alkali oxides in the

Jan 1, 1949

By C. E. Lesher

COAL has been fighting a rear-guard action since the last World War. The battle against competitive fuels has been largely guerilla warfare with more sniping within the ranks than of organized opposition. Oil and natural gas are the fuels that over these twenty odd years have driven coal backward and out of many profitable markets. Now, somewhat timidly, the coal industry is trying a new weapon; namely, Research, or let us more properly say, Organized Research. Engineers have been designing this weapon for many years, supported by those interested in coal, including some coal producers. A part of this pioneer work has been Fundamental Research, the Ph.D. kind that is over the heads .of most of us. Another part has been aimed at immediate objectives and realizable profits, the practical, man-in-the-street sort. That is Industrial Research. Enough has been accomplished to make a fair exhibit, but whether this new weapon will have sufficient fire power to rout the opposition, whether the industry will really go into production and use it, the next few years will tell. NEED FOR COAL RESEARCH To utter "Research" is to use the modern magic word; to conjure up the miraculous-rubber from weeds; radar; magnesium from sea water; yes, even gasoline from coal. Research is a very general term. It means something different to every man. What is the coal industry seeking with its research; or what should it seek? And, specifically, how is it going about the job; and is it taking the best way? There are many who say that Coal has been asleep at the switch, while Oil and Gas have been taking the energy business. In an organized way this is true. Large-scale, privately financed research is just started in the Pennsylvania, anthracite industry, and it is still a dream for bituminous coal. What has been done so far collectively is purely defensive; as, for instance, to improve mechanical devices for burning coal so as to be able to recover markets for house-heating fuel long since abandoned to oil and gas. To appreciate just how seriously bituminous coal has slipped back in the national economy in the past 25 years, one has only to recall that, in the last war the Navy required for its operations all the high-grade, low-volatile coal that could be produced, and that anthracite was withdrawn from the middle and northwest markets to keep the eastern seaboard warm. All coal was "rationed" by zones, if not to individuals. Now the Navy, the Armed forces and the Merchant Marine are propelled by oil and gasoline. Gasoline and heating oil are rationed to individuals. Production of all coal in this country in 1918 reached the historic figure of 678,200, 000 tons, and in 1943, after 25 years, it is expected to reach a special wartime total of 660,000,000 tons. Meanwhile, production of crude oil this year may exceed 1,500,000,000 bbl., and like that of natural gas, reach four times the amount produced in 1918.

Jan 1, 1944

By E. E. Donath

THE coal hydrogenation process is well known as a means for the production of liquid fuels -from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aromatics and of tar acids and tar bases. The relative amounts of heavy and middle oil-boiling above and below, e.g., 325°C-can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.1 Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydro¬gen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catch-pot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1952

By J. E. Gould, H. J. Hand

Many independent studies are being made on slag-metal relationships in the open-hearth furnace, and these studies cannot help but result in an ultimate improvement in the quality of open-hearth steel of both the open and killed types. In maintaining quality control at the National Tube Company's plant, emphasis has been placed on an evaluation of the iron oxide content of the steel in as quantitative a manner as possible, in order that the most desirable level of oxidation might be obtained for a given type of steel, and to secure a more precise basis for final de-oxidation. In the past, various methods were used for estimating FeO content of the metal at tap to ensure uniform and thorough deoxidation of killed steel, avoiding overdeoxidation to minimize the amount of inclusions present and to make as sound a steel as possible. For the open-type steels, such control involves obtaining the necessary level of oxidation for the most suitable action of the steel in the molds to provide good surface quality and cross section for the specific grade involved. While rapid analytical methods are available for determination of FeO in the liquid metal, such methods are still not sufficiently rapid for routine control on the open-hearth floor, nor do such analyses provide information as to what causes high or low FeO values. The method of sampling can still be considered a problem in view of the variability encountered in taking simultaneous duplicate tests. With the accurate rapid methods now available for determining carbon in the metal, estimating slag basicity and obtaining temperatures of liquid metal, it was believed possible to determine the influence of the various furnace reactions in establishiug the state of oxidation at a given time. Simultaneous slag and metal tests were used in this analysis, aided by statistical methods, to determine the factors that affect the metal FeO, and also to make a quantitative evaluation of these factors. Data obtained are from actual iurnace operations, the metal test being of the I spoon, Herty type, and taken in duplicate. Metal temperatures were taken with the open-tube bath pyrometer developed by the Research Laboratory of the United States I Steel Corporation. This method of taking open-hearth metal temperature was invented by Collins and Oseland,l and was developed into its present form by L. 0. Sordahl,2 of the Research Laboratory. The instrument and its mode of operation have been fully described by Sordahl and Sosman in three publications.3,4,5 lag components were obtained by chemical analysis. Data were taken from four 165-net-ton furnaces during the working period of the heat. Recognizing that additions of ore affect the metal FeO. no tests were included within 30 min. after ore additions. In all, 65 tests (48 heats) were used in this study.

Jan 1, 1942

By D. H. Turner, F. A. Crossley

The titanium-rich corner of the system Ti-Al-Si has been studied to determine the phase relationships in the temperature interval 600° to 1200°C. Metallographic examination of long time isothermally annealed specimens was the means of investigation. PART of a program on phase relations and transformation processes of titanium alloy systems included the study of the titanium-rich corner of the Ti-Al-Si system. The investigation covered ternary compositions in the range 2 to 8 pet A1 and 0.1 to 2 pet Si and binary compositions in the range 0.2 to 2 pet Si. Temperatures were in the range of 600" to 1200°C. Alloys containing 6 pet A1-0.1 to 0.5 pet Si were investigated down to 400°C. Partial vertical sections are presented for 2, 4, 6, and 8 pet Al. The Ti-Si system has been reported by Hansen et al.' It is characterized by a eutectoid decomposition, ß = ± a + Ti3Si3, at 860°C. The maximum solubility of silicon in a is reported to be about 0.5 pet at the eutectoid temperature. The solubility of silicon in 0 increases from 0.9 pet at the eutectoid temperature to approximately 3 pet at the eutectic temperature, 1330°C. Several investigations in the composition range of interest have been reported for the Ti-A1 system."' These investigations are in agreement on the phase fields, but differ to small extents on boundary positions. However, very recent, and as yet unpublished, findings" " indicate that there are perhaps two phases which occur at lower aluminum contents than the ? (TiA1) phase, and that the solubility of aluminum in a titanium is less than 6 pet. In the present investigation phase relations found are in agreement with the published literature exemplified by the work of Bumps et al.3 Therefore, it is probable that the partial system reported herein is metastable and does not represent true equilibrium. Experimental Procedure High purity Bureau of Mines titanium sponge of 103 Bhn hardness, granulated aluminum shot of 99.7 pet purity, and silicon powder of 99.8 pet purity were used in making the alloys. For the work in the range from 600" to 1200°C, 100 g ingots were prepared by arc melting. Melting losses were negligible and spot checks by chemical analysis showed good agreement between nominal and analyzed results. Nominal compositions are used throughout this paper. Ingots were forged to 3/8 in. rounds and cut into specimens for heat treatment. Isothermal anneals in the range from 600" to 900°C were preceded by solution treatment at 1000°C for 1 hr, followed by furnace cooling to the annealing temperature. Samples were sealed in evacuated Vycor bulbs for heat treatments up to 1000°C. Higher temperature anneals were done with the samples sealed in quartz bulbs under a partial pressure of argon.

Jan 1, 1959