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By H. E. Howe, A. A. Smith

The creep properties of lead alloys have been studied by a number of investigators but most of the work has been done on extruded material and the amount of data available on rolled alloys is surprisingly limited. Greenwood1 and his collaborators investigated various rolled commercial leads containing relatively small amounts of impurities, Phillips2 likewise studied rolled commercial leads, although he did include a few alloys— such as tellurium lead and one per cent antimonial lead. But as far as the authors are aware no data on the creep properties of so-called "hard leads"-—i.e., containing from 4 to 8 per cent antimony—have been published. In this paper some data are presented on a few antimonial lead alloys and compared with a copper-bearing lead. Preparation OF Specimens All the alloys used in this investigation were cast at a temperature of 400°C. into an open cast-iron mold preheated to Ioo°C., the resultant casting being % by I by 10 in. The copper-bearing alloy was cold-rolled by 10 per cent passes to a thickness of 0.100 in. Creep specimens 16 in. long were prepared by clamping the strips between wooden blocks and machining the edges of the strips parallel by means of a plane. Careful manipulation gave parallel specimens with no reduced section and with a minimum of distortion. The antimonial lead castings were hot-rolled in 10 per cent passes at a temperature of I50°C. to a thickness of 0.400 in., the heating being carried out in an electric oven after each pass through the rolls. After the castings had been broken down to 0.400 in., they were allowed to cool to room temperature and then cold-rolled to 0.100 in. with the usual Io per cent passes. Sufficient time was allowed after each pass for the strips to cool to room temperature. The apparatus and method of measuring strain have been adequately described in a previous paper3 and essentially the same practice was used in obtaining the present data. Time-extension curves for only two alloys are given, since these are typical of all. Figs. I and 2 show the time-extension Curves for the copper-bearing alloy A at 30°C. and loo°C., and Figs. 3 and 4 show

Jan 1, 1945

Discussion of the paper of O. P. Hood, presented at the Pittsburgh meeting, October, 1914, and printed in Bulletin No. 94, October, 1914, pp. 2607 to 2611. R. V. Norris, Wilkes-Barre, Pa.-I have had a little experience with gasoline locomotives and I want to indorse very strongly Mr. Hood's point with regard to the danger of carbon monoxide poisoning. I think .the terrible danger is not fully realized. I was foolish enough some time ago, in investigating a gasoline locomotive, to attempt to walk out of the mine entry behind it, and for several days I felt very seriously the carbon monoxide effects. The use of gasoline locomotives ought to be confined to mine entries where there is a very large amount of air. One of the grave dangers is their great convenience and the temptation to run them into chambers for just a few moments to get a car or two. GEORGE S. RICE, Pittsburgh, Pa.-Apparently one of the great dangers is in the style of the gasoline engine. When my attention was. first directed to the type of gasoline locomotives which I saw in the foreign mines-France, Belgium, and Germany, I was most favorably impressed with them, and they have given no trouble on account of fumes, so far as I could learn. Large numbers of them were being used, but all were of small capacity, and of a kind in which the speed control is by a governor of the hit-or-miss type, the engine running continuously. Their power capacity was very low, if I remember correctly it was not over 4 or 5 h.p., but they were used under favorable conditions where the grades in the mines were slight, since the entries or tunnels bad a slight grade in favor of-the load, making about the same pull for the empties against the grade as for the load with the grade. I understand the hit-or-miss valve arrangement enables a setting that will give more perfect combustion than can be insured with the valve controlled by the operating man, as in the automobile type of valve and engine used in this country. Apparently the European type of locomotive does not have the capacity to permit use under the conditions existing in this country, where most of our entries or tunnels have variable grades and long heavy trips of mine cars are used.

Jan 4, 1915

By G. R. Countryman, G. H. Thomas, I. Fatt

Miscible displacement in both thewetting and non-wetting phase has been studied in two-phase systems. Experimental data show that dispersion is a function of saturation and cannot be predicted from dispersion theory developed for single-phase miscible displacement. Some of the effect of saturation on dispersion is a result of the development of dead-end pores or a dendritic pore structure in multiphase systems. The presence of dead-end pores or dendritic structure is confirmed by pressure transient studies. INTRODUCTION Displacement by flooding with a miscible liquid is a possible means for recovering the estimated two-thirds of the oil that remains behind after primary production. The immense economic importance of a process that can recover such large quantities of oil has led to extensive laboratory studies of miscible displacement. As usual in production research, most laboratory studies of miscible displacement have not attemped to reproduce all of the conditions existing in a petroleum reservoir. In the early stages of investigation the need has been for information on the broad, basic principles of the phenomena involved in miscible displacement. The effects of overburden pressure, reservoir temperature, and wettability have been considered of secondary importance. However, one property of a petroleum reservoir which is expected to be of major importance and yet has been omitted from many laboratory studies is the presence of interstitial water. Two possible effects of interstitial water on the displacement mechanism in the hydrocarbon phase immediately come to mind. First, from the general1y accepted theory that capillarity governs the distribution of oil and water in porous rock one would expect that for water-wet rock the water will be in the small pores and oil in the large pores. A miscible displacement of oil carried out in the presence of water is operating in a pore size distribution shown in Fig. lb, whereas if the same test had been performed with only one phase present the pore size distribution is as shown in Fig. la. Although there is not yet a theory of miscible displacement which explains in detail the effect of pore size distribution, one would expect the differences between Figs. la and lb to influence the displacement efficiency. A second factor which may make a multiphase system different from a single-phase system is the presence in the multiphase system of dead-end pores or dendritic structure. Experiments of various kinds on reservoir rock have led to the belief that all pores in the network structure of a porous rock take part in conducting fluid during single phase fluid flow.1,2 There are then no dead-end pores and no fingers or dendritic structures containing stagnant fluid. In a multiphase system, however, the second phase may

THE Institute assembled on Tuesday evening, in the building of the University of Pennsylvania. In the absence of President Thomas, Vice-President Raymond occupied the chair. The Institute was welcomed in an eloquent and thoughtful address by Prof. J. P. Lesley, to which Mr. Raymond responded. Invitations were announced from the proprietors of Sellers' Tool Works, Whitney's Car-wheel Works, the Baldwin Locomotive Works, Lewis & Brothers' White Lead Works, the Southwark Foundry, Harrison's Boiler Factory, the University of Pennsylvania, and the Academy of Natural Sciences. The following gentlemen, being duly recommended by the Council as members and associates, were unanimously elected : Alexander, John S., . . . . . Philadelphia, Pa. Biddle, E. R., . New Pork. Britton, J.. Blodget, . . . . . Philadelphia, Pa. Brooks, Maj. T. B., . . . . . Marquette, Mich. Brown, D. P., . Pottsville, Pa. Canfield, Edw., . . . . . . Dover, N. J. Cogswell, W. B., . .Franklin IronW'ks, N. Y. Cornwall, Prof. H. B., . .New York. Edwards, Daniel, . . . . . . Danville, Pa. Estabrook, Juhn D., . . . . . Philadelphia, Pa. Firmstone, William, . . . . . Easton, Pa. Fritz, John, . . . . . . . Bethlehem, Pa. Gignoux, Charles, . . . . . . New Pork. Grant, E. M., . . . . . . . Tuskegee, Ala. Humphreys, A. W., . New York. Ingham, W. A,, . . . . . . Philadelphia, Pa. Keyes, W. S., . . . . . . Eureka, Nev. Kimball, Dr. J. P., . New Pork. Law, Charles, . Pittston, Pa. Neilson, W. O., . . . . . . Philadelphia, Pa. Newberry, Prof. J. S., . . . . . New York. Pearse, John B., . .Steel Works P. O., Pa. Ricketts, P. De P., . . . . . New Pork. Scranton, Col. Charles, . . . . . Ox ford, N. J. Sontag, Hugo, . . . . . . Cologne, Prussia. Steele, Thomas C., . .Summit, Pa. Wharton, Joseph, . . . . . . Philadelphia, Pa.

February 20th, 1872. THE Institute assembled on Tuesday evening, in the building of the University of Pennsylvania. In the absence of President Thomas, Vice-President Raymond occupied the chair. The Institute was welcomed in an eloquent and thoughtful address by Prof. J. P. Lesley, to which Mr. Raymond responded. Invitations were announced from the proprietors of Sellers' Tool Works, Whitney's Car-wheel Works, the Baldwin Locomotive Works, Lewis & Brothers' White Lead Works, the Southwark Foundry, Harrison's Boiler Factory, the University of Pennsylvania, and the Academy of Natural Sciences. The following gentlemen, being duly recommended by the Council as members and associates, were unanimously elected Alexander, John S., - Philadelphia, Pa. Biddle, E. R., - New York. Britton, J.. Blodget, - Philadelphia, Pa. Brooks, Maj. T. B., - Marquette, Mich. Brown, D. P., - Pottsville, Pa. Canfield, Edw., - Dover, N. J. Cogswell, W. B., - Franklin IronW'ks, N.Y. Cornwall, Prof. H. B., - New York. Edwards, Daniel, - Danville, Pa. Estabrook, John D., - Philadelphia, Pa. Firmstone, William, - Easton, Pa. Fritz, John, - Bethlehem, Pa. Gignoux, Charles, - New York. Grant, E. M., - Tuskegee, Ala. Humphreys, A. W., - New York. Ingham, W. A., - Philadelphia, Pa. Keyes, W. S., - Eureka, Nev. Kimball, Dr. J. P., - New York. Law, Charles, - Pittston, Pa. Neilson, W. G., - Philadelphia, Pa. Newberry, Prof. J. S., - New York. Pearse, John B, - Steel Works P. O., Pa. Ricketts, P. De P., - New York. Scranton, Col. Charles, - Oxford, N. J. Sontag, Hugo, - Cologne, Prussia. Steele, Thomas C. - Summit, Pa. Wharton, Joseph, - Philadelphia, Pa.

Jan 1, 1873

By A. L. Bailey, B. A. Landry

W. W. ANDERSON and G. E. KELLER*—We want to compliment the authors on this very thorough paper. It gives information which the coal industry has needed for some time. We hope that the additional information which the authors are collecting will he available shortly. The mixing and riffling procedure that was followed for experimental purposes is obviously not practical in routine float-and-sink testing because of the particle size degradation which would result in handling the sample so many times. It is important to obtain our tloat-and-sink fractions with a minimum amount of handling of material. A statement is made in the paper (p. 80) that "the variable most likely to affect the size of sample required to meet a given preassigned accuracy would be the state or degree of mixing of the coal." We agree that this is a large factor, but do not believe it is the most important factor. Our own opinion is that the most important single factor governing the total gross weight of sample that must be collected is the percentage of the weight of material in the smallest fraction that results from the screening and float-and-\ink operations. In other words, size of sample is governed by the total number of fractionations that must he made, and the distribution of material within the fractions. We can imagine a coal with perfect mixing, but with such a small amount of material in some float-and-sink fraction in one of the coarse sizes that a much larger sample would have to be taken than would be the case with very poorly mixed material, but with a large percentage of coarse material more evenly distributed in all float-and-sink fractions. Our own observation of many float-and-sink tests that we have run in our own organization on many types of coal is that the size of sample that must be used on fine size float and sink is governed more by the requirements for weight of material to be used for analysis in the laboratory than by weight of material necessary to obtain accurate float and sink percentage of weight values. In other words, it is our opinion that very small samples can be used for float-and-sink fractionation in the fine sizes, but that accurate analysis of the fractions will depend on a larger weight of sample being pulverized for the laboratory than is necessary to establish the float-and-sink distribution with respect to weight. A. L. BAILEY and B. A. LANDRY (authors' reply)—The authors thank Messrs. Anderson and Keller for their comments based on long experience. It is agreed that the involved mixing and riming technique used may be disadvantageous from the standpoint of degradation. Fortunately, the paper does point out that the extended riming was unrewarding in causing further mixing. Two large unknowns remain, however: (1) how much of the mixing from the presumed highly unmixed state in the bed was achieved toward the random state during blasting, loading, transportation, screening, and further transportation to the point where the gross sample was taken, and (2) how much of the mixing took place during the preparation described preceding riming. As has been pointed out by one of the authors.6 the degree of mixing has a very large effect on the size of sample required and there are still too few experimental data to show at what stage of coal handling most of the mixing occurs. The discussion states that the weight of material in a screened fraction, or in a float-and-sink fraction, is more important than the mixing factor. We do not believe that these factors are comparable in this instance inasmuch as our purpose was to give minimum sampling requirements to achieve a preassigned accuracy in the percentages of float, middlings, or sink, and nothing more. The gross sample had already been screened and no further division by screening was made or contemplated; also, it was not intended that the middlings and sink fractions would necessarily be adequate for percentage ash or other determination. In other words, the sample obtained by the method outlined is not intended for washability studies but only for preparation plant control. Further experimental work has been done, since the paper was prepared, to investigate the effect of increasingly larger top and bottom sizes on the variability of float, etc., of a double-screened coal from Western Pennsylvania. Results will be published and eventually attention is to be given to the preparation of sampling specifications. E. H. M. BADGER*—I should like the authors to explain more fully the fundamental assumptions on which their Eq 4 is based. The equation is of the form s2 = p(l - p) which is the usual expression for the (standard deviation)2 when the chance of finding a particular kind of particle in the sample is proportional to the number fraetion, p. But instead of the number fraction, the authors have used the weight fraction, WF/W. The chance of finding a particular kind of particle in the sample can only be proportional to the weight fraction, if the average ?eig?ts of all kinds of particles, that is, float, midlings, or sink, are the same. Surely a much more justifiable assumption would be that the average volumes of the particles are the same, and, if this is so, Eq 4 would not be true. This may be demonstrated as follows: Let be the weight fraction of float, middlings, or sink, dl the density of this fraction, and d2 the density of the rest of the coal. Then assuming that the average volumes of the pieces in the three classes are the same, the number fraction, p, is given by ? P = d1/l-?/d2 + ?/d1 = ?d2/d1 + ?(d2-d1) The weight fraction, w, in terms of p is given by ? = pd1/(l-p)d2 + pd1 = pd1/d2 + p(d1-d2) _____ [61

Jan 1, 1950

By C. A. Stickels, C. M. Yen

Secondary recrystallization was investigated in vacuum-melted electrolytic iron to which 70 pm N was vacuum-meltedadded. The secondary texture is "near {554}<225>" for material cold-rolled 75 to 90 pct, the sharpness of the texture increasing with increased rolling reduction and with decreased annealing temperature. At reductions of 95 and 97.5 pct the secondary texture is &apos;"near {322)(296)". Both secondary orientations also exist as major components of the primary re-crystallization texture. Development of a strong "near {554) (225)" secondary texture appears to depend on the evolution of the Primary texture to a transition texture depleted in orientations near the secondary orientation before the onset of secondary growth. A variety of qualitative experinzents have been used to show that nitrogen is important in limiling primary grain growth. The presence of nitrogen does not seem essential for the establishment of a transition texture, but a loss of nitrogen during annealing may facilitate growth of grains in the secondary orientation. Secondary grains we shown to form initially at the specimen surface. This is not thought to indicate that surface energies are important in the growth process. It is proposed that the quasi-two-dimensional character of surface grains permits discontinuous growth parallel to the surface before secondary growth of interior grains is possible. An earlier study of recrystallization textures in 90 pct cold-rolled electrolytic iron showed that secondary recrystallization occurred after annealing for several days at 700C1 This type of secondary recrystallization, which had not been reported previously, results in the formation of a strong texture, best described by the indices "near {554}(225)". The purpose of the present work was to investigate the effect of various processing variables on secondary recrystallization in this material and determine the mechanism of secondary grain growth. LITERATURE REVIEW An understanding of the mechanism of a secondary recrystallization process depends on knowing: 1) how grains in the secondary orientation come to be in the primary recrystallization texture; 2) why normal grain growth does not occur; and 3) what factors determine the strength of the secondary texture. For secondary growth of grains of a particular orientation, a certain minimum fraction of the grains must be in that orientation after primary recrystallization. This requirement is apparently satisfied "naturally" in certain systems, i.e., when the primary texture obtained by rolling and recrystallizing material initially randomly oriented contains a sufficient fraction of primaries in the secondary orientation. However, in other cases, e.g., {110}<001> and {100}<001> secondary growth in silicon iron,2 it is necessary to enhance the fraction of primary grains in the secondary orientation by rolling and recrystallizing textured material. In the present case, the "near {554}<225>" orientation is contained within the spread of orientations found in the primary recrystallization texture of iron or bbc iron-base alloys. In systems where the main driving force for secondary growth is the reduction in total grain boundary energy, secondary growth is observed only when normal grain growth is minimized. Four ways in which normal grain growth can be limited are: 1) Limitation by a strong primary texture. When a very strong primary texture consisting of a single component or twin-related components develop, most primary grains are separated from one another by relatively immobile small-angle grain boundaries. The classic instance of this is secondary growth into the primary cube texture in some fcc metals. 2) Limitation by precipitates. Precipitates present in the proper volume fraction with a suitable dispersion will limit primary grain growth. The role of MnS inclusions in impeding normal grain growth in Si-Fe is well-documented.5 3) Limitation by sheet thickness. Normal grain growth slows drastically when the mean grain diameter is of the same order as the sheet thickness. This effect has been used to obtain secondary recrystallization in thin sheets of high-purity silicon iron.&apos; 4) Limitation by solute impurities. It is well-established that certain impurity elements in solution can have a large effect on grain boundary mobility.&apos; However, there does not seem to be any secondary recrystallization process in which primary grain size stabilization has been shown to be due to the drag exerted on grain boundaries by dissolved impurities. In certain systems, e.g., secondary recrystallization in silver,&apos; the means by which normal grain growth is limited has not been identified, and solute-impurity limitation might be suspected. In order to understand the factors which determine secondary texture strength in three-dimensional growth, it is necessary to examine in more detail the current picture of general secondary recrystallization processes. Following Cahn,9 it is assumed that the primary grains have a range of sizes and that secondary growth of one of the large grains in this distribution is possible when it exceeds a critical size with respect to its neighboring grains. The critical size depends on the ratio ?S/?p, where ?s is some sort of average grain boundary energy between the potential secondary and the primary grains and ?p is some sort of average grain boundary energy between primary grains. For a constant primary grain size, the critical size for secondary growth increases as ?$/?p increases. May and Turnbull5 have incorporated the

Jan 1, 1969

By J. B. Wagner, p. Hembree

The iron tracer diffusion coefficient of umstite has been measured at 110(fC across the phase field and at a single composition at 800°C. Assuming a simple cation vacancy model the tracer diffusion coefficient was found to be a linear function of the cation vacancy concentration at 1100°C. The equation is D = 3 x 20 29 where denotes the concentration of vacancies in numbers per cc. The tracer work at 800°C was carried out to investigate the reported "pinning" of tracer to the wustite surface at low temperatures. No evidence for the "pinning" of the tracer was found at 800°C in COz-CO gas mixtures. HIMMEL, Mehl, and Birchenall,&apos; Carter and Richardson,2 and Desmarescaux and La combe3 have measured the diffusion of iron tracer in wustite at several temperatures and compositions. The present work was undertaken to extend the measurements over a large composition range at 1100°C and to resolve certain apparent discrepancies in the data, expecially at lower temperatures. EXPERIMENTAL Wustite was prepared by oxidizing rectangular iron plates* in C02-CO mixtures. The samples were •The iron was supplied by the Battelle Memorial Institute courtesy of the American Iron and Steel Institute. The analysis is presented in Table I. quenched. Due to the inward flow of cation vacancies during oxidation, the center of the sample contained a thin void. The edges of the wustite slab were sanded until the sample could be split into two parts. Each part was then sanded on the front and back flat area until a smooth surface was obtained. The specimens were then replaced in the furnace and equilibrated at llOO°C in a predetermined COa-CO mixture by methods described elsewhere.4"6 The specimens were again quenched and the surfaces were lightly sanded to remove any roughness following the first equilibration. The specimens were then reequi lib rated in the same C02-CO mixture for thirty minutes in order to relieve any mechanical damage on the surface due to the polishing. The specimens were then quenched and the tracer was applied by an electroplating technique. The work of Carter and ~ichardson&apos; demonstrated that there was no systematic difference in the iron tracer diffusion coefficient in wustite if the tracer was plated, dried, or evaporated on the specimen. In the present study a piece of filter paper was saturated with an iron chloride solution of pH <* 3 that contained the tracer FeS5. The wustite was placed on the filter paper and made the cathode. A current density of 0.4 to 0.6 ma per sq cm was passed for about five to ten minutes. The thickness of the tracer layer was estimated to be about 7 x lom6 cm. This estimate was made by considering the area plated, the current flow, and time for plating and the activity of the iron in the plating solution. Different areas of the specimen were counted using a collimator to determine the uniformity of the tracer. Any specimen which exhibited a variation from the initial count rate (about 1500 cpm) by more than 15 pct was rejected. An estimate of the time necessary to convert the thin layer of iron tracer to wustite was made using the data of Pettit and wagner." he estimated time was 1 sec at 1100°C assuming linear oxidation kinetics. The shortest diffusion anneals were 1800 sec. The samples were suspended in the hot zone of a furnace by two platinum wires. Two separate specimens were run at the same time. Only the edges of each sample were in contact with the wires. The C02-CO gas of the same composition as that used in the pre-diffusion anneals flowed freely around the samples at a linear velocity of 0.9 cm per sec. To initiate a run, the specimens were lowered from the cold zone of a furnace to the hot zone by a magnetic lowering device." bout 60 sec were required for lowering. To terminate a run, the sample was withdrawn from the hot zone to the cold zone. Time zero for the beginning of the experiment was taken when the sample blended into the red glow of the furnace and conversely for the end of the experiment. The surface decrease method of measuring the tracer diffusion coefficient was used to collect the data. This method requires that counting geometry be reproducible because the specimen is counted before the diffusion anneal and after the anneal. A special jig was constructed for each specimen so the specimen could be removed from the jig and returned to the jig such that the well geometry was reproducible.

Jan 1, 1970

By E. A. Gulbransen, W. S. Wysong

The behavior of molybdenum and its surface oxides in oxidizing and reducing gas atmospheres and in high vacua at elevated temperatures is a question of scientific and technical importance. The use of molybdenum as a metal or as an important component in alloys in oxidizing atmospheres at elevated temperatures has been limited because of the unprotec-tive nature of its oxide film and the volatility of this oxide at moderate temperatures. This communication will present results of a vacuum microbalance studyl, 2 of the following problems: (I) the oxidation kinetics in the temperature range of 250°to 450°C; (2) the reduction with pure hydrogen of thin oxide films formed on molybdenum; (3) the volatility of the thin oxide films; and (4) the vacuum oxidation of molybdenum at high temperatures. Molybdenum is an interesting metal to study for the following reasons: (I) although the oxide-to-metal-volume ratio is greater than one, the metal is not considered protective; (2) the metal oxidizes readily at temperatures of 2 50°C and higher; (3) the oxides of the metal are reduced at temperatures as low as 500°C by pure hydrogen; (4) the oxide Moo3 melts at 795°C; and (5) the oxides of molybdenum are volatile at moderate temperatures. The following variables are studied in the oxidation kinetics: time, temperature, pressure, surface preparation, surface area, concentration of inert gas in the lattice, cycling procedures in temperature, vacuum effect and high temperature vacuum oxidation. The general interpretation of many of these factors has been previously discussed. Literature The oxidation of molybdenum has not been studied critically. Although many studies have probably been made on the kinetics of the oxidation process, none has been reported in the literature available to us. The crystal structures found in the oxidation of molybdenum have been studied by Hickman and Gulbransen." Their results showed that Moo2 is the oxide which is stable in contact with the metallic substrate throughout the temperature range 300 to 700°C. As the film thickens in the low temperature range, MoO3 becomes predominant on the surface. Above 400°C, Moos is no longer observed, MoO2 being the only oxide found. Hagg and Magneli6 have shown from an X ray study that the a-phase, orthor-hombic Moo3 is stable up to 1050°C. Two other phases, ß and ß with compositions close to MoO2.90 are also obtained. The formula for the 0 phase is not given but that of the ß phase is defined as Mo9O26 The 0&apos; phase is found to be built upon a monoclinic unit cell. A ?-phase is isolated from a preparation MoO2.75 heated for 17 hrs at 670°C. This phase is

Jan 1, 1949

By N. B. Wittman

The working of blast-furnaces is always of interest to many members of the Institute, for which reason I present an account of the working of the furnaces of the E. and G. Brooke Iron Company, of which I have had charge for the past four years. Although there are no phenomenal runs to record, there have been long periods of satisfactory work, and also periods—altogether too long—when one of our furnaces has behaved in a way which may be described as "nagging." All the conditions were apparently normal,but only a very light burden could be carried, which of course resulted in a high fuel-consumption to the ton of iron, as well as increased cost of labor. The two active furnaces of this company have the following dimensions and equipment : No 2. No 3. Feet. Feet. Height ....55 60 Diameter at bosh,.....- 15, 16 " hearth,...... 8 74 " stock-line,..10 91/2 Height of bosh,..23 23 " tuyeres,. 5 5 Diameter of bell,.7 6 Front,....closed open Both furnaces are blown with I. P. Morris condensing-engines, sim

Jan 1, 1890

By Y. H. Liu, R. Kiessling

The chromium, iron, and tungsten borides have been treated with ammonia at different temperatures. They are attacked, forming metal nitride and boron nitride, and the results are summarized in the tables. In the tungsten-nitrogen system a new phase has been observed, closely related to the known ß phase. THE present investigations were begun to determine whether any ternary phases exist in the transition metal-boron-nitrogen systems for the metals chromium, iron, and tungsten. Attempts to prepare such phases were made by using the borides of the metals as starting materials and ammonia as the nitriding agent. Although no new ternary phases have been found to exist, the results may be of some interest with regard to the technical use of the borides. General Procedure A steady stream of dry ammonia was passed through a silica reaction tube, the central part of which was kept at the reaction temperature while its ends were water-cooled. Weighed amounts of the borides were placed in a silica or porcelain boat and heated at different temperatures for a period of 10 to 24 hr. The boat was then rapidly removed from the reaction zone to the quenching zone, the water-cooled end of the tube, by means of a simple magnetic device. The nitrogen content of the products was determined by the increase in weight of the specimens, and the phase analysis was carried out by X-ray methods. For this analysis a Guinier-type camera, constructed at this Institute, was used with a bent, ground quartz crystal monochromator. The general reaction, which occurred in all the experiments, may be summarized as: metal boride + nitrogen -* boron nitride + metal nitride For the higher temperatures pure metal was formed instead of metal nitride. It is sometimes difficult to Discussi detect boron nitride among the reaction products by X-ray methods. Prolonged exposures of some specimens showed, however, that the strongest reflections of boron nitride were present. Additional evidence for its presence was given by the increase in weight of the specimens after nitriding. This increase was always greater than that corresponding to nitride formation only and was often in close agreement with the formula given above. Finally, a white powder, which was shown by X-ray methods to be boron nitride, was left if the reaction products after nitriding Fe,B at 448°C and FeB at 768°C were dissolved in diluted sulphuric acid. Ch rom iu m - Boron - N itrogen Five phases have been found to exist in the Cr-B system,&apos; , and all were used as starting materials. Investigations on the Cr-N system have shown the existence of two nitrides with ideal composition Cr,N and CrN.".&apos; * The results are summarized in Table I. All the borides are attacked and decomposed into chromium nitride and boron nitride, and the kind of nitride formed depends only on the temperature and not on the boride used as starting material. The lowest reaction temperature, however, is different for the different borides. Thus the 6 phase begins to react at about 735 "C, the r phase at about 800°, the S phase at about 900°, the 7, phase

Jan 1, 1952

By F. J. Tuck

THE Hayden mill of the Ray Mines Division, Kennecott Copper Corporation, is now equipped with two 9 by 12-ft. rod mills having a daily capacity of 6000 tons of coarse-crushing plant product from the mine. These two mills crush a ¾ -in. product to approximately 19 per cent on 14 mesh, with only one pass through the mills. Each rod mill has taken the place of four sets of 42-in. Garfield rolls with their attendant screens, and is making a product for the fine-grinding department comparable to that formerly made by rolls in closed circuit with screens. The rod mills are lined with wave-type liners of white iron, varying in thickness from 2 to 3 in. The shell and end liners last approximately 600 to 700 days. Manganese-steel lifter bars, 3 5/8 in. thick, are used, spaced about 11 in. apart, and they give a life of 350 to 450 days. Fig. 1 shows the general design and thickness of the wave-type liners and lifter bars; 1 ½ -in. liner bolts are used to fasten the lifter bars to the shell. The shell liners are held in place by the tapered lifter bars. A 3/4-in. wood backing is used between the shell and the liners. The rod-mill scoop has removable manganese-steel lips, which last 250 to 300 days. The scoop proper has shown some wear in spots, and these spots have been protected by rubber bolted over them. Water and milk of lime are added to the elevator feeding the mill, but not enough water to cause a pounding of the rods against the shell. Roughly, the water added amounts to 25 to 33 per cent of the ore. Additional water is added to the mill discharge to facilitate distribution to the classifier bowls in the fine-grinding department. Rods are charged to the mill once every four days, the mill being down about 20 min. for this purpose. Other delays are negligible, and usually are due to a loose liner bolt or possibly power trouble. However, these occasions are extremely rare. In charging the mill, a crane is used

Jan 1, 1938

The present paper records a chapter in the history of the development of an electrolytic manganese industry in the United States.l A relatively large pilot plant at Boulder City, Nev., for the production of electrolytic manganese was conceived as part of the national defense program to make this country independent of foreign importation of manganese ore. The first authorization, in November 1940, however, was for a plant of only several hundred pounds capacity. Improvements in process and subsequent additions to some sections authorized by subsequent appropriations have enabled the plant to produce as much as 2000 lb. of manganese a day for substantial periods of time. Since in pilot-plant operation frequent changes are made in the flowsheet, the electrolytic manganese plant was constructed so that equipment could be rearranged with a minimum of expense and time. Several different kinds of the various ¦ types of equipment were installed for many of the operations, so that the one most suitable for the process might be chosen. Pilot-plant operations were begun in November 1941 and have been continuous except for brief shutdowns for installation of new equipment. More than one-half million pounds of manganese have been produced. The improvements in process, selection of equipment, and operational procedure developed are recorded here. Development of the Process The work of early investigators on the electrolysis of manganese solutions has been reviewed by Shelton. Until the method of continuous production of manganese by electrolysis was perfected by SheltonZm4 and coworkers, no practical procedure had been devised. The method as originally developed by the Bureau of Mines will be described here only briefly. The manganese dioxide ore was reduced in a rotating kiln-type furnace at 650°C. in an atmosphere of "city" gas. The calcine was leached with spent electrolyte and enough sulphuric acid to produce a neutral leach solutioil containing 2 5 grams manganese per liter as manganese sulphate and zoo grams per liter of ammonium sulphate. Arsenic was removed from the solution by the addition of 0.0j gram iron per liter as ferrous sulphate followed by oxidation with manganese dioxide, and aeration, which precipitated the iron as ferric hydroxide. The solution, free from iron

Jan 1, 1944

By F. A. Schaufelberger

METAL can be recovered from a leach solution either indirectly by precipitation as a compound that is later reduced or directly by electrolysis, cementation, or chemical reduction, for example, with hydrogen. The widely used electrowinning processes suffer from the inefficiency of converting fuel to low voltage dc and from low current efficiency when complete recovery is attempted. With the batch hydrogen reduction methods outlined here, a unit of fuel converted to hydrogen in modern gas reform plants will make two to three times as much metal as can be obtained with electrolysis. With continuous hydrogen reduction, four to six times as much metal is obtained. Precipitation by reducing a metal salt solution with H, has been known for almost 100 years.&apos; Commercial use of the process, however, awaited the research and development program initiated by Chemical Construction Corp. Within the last few years this program has brought about construction of commercial plants, listed on page 545. Ideal hydrogen reduction will precipitate a pure metal from a solution obtained by commercial leaching methods at a rapid rate without excessive temperatures and pressures. The metal precipitate will be of desired size and density, less than a percent left in the vessel being deposited on the wetted parts. The present discussion will outline Chemical Construction Corp.&apos;s early development program and will discuss the chemistry and mechanics of reducing copper, nickel, cobalt, and cadmium from solution by H2. Work on selective reduction of nickel from cobalt has been described earlier.&apos; The article is not concerned with precipitation of copper by disproportionation of cuprous solutions where yield is limited3 to 50 pet.* It does not discuss use of gaseous reducing agents other than hydrogen, such as SO2,4 which may lead to contamination with sulfur, or C0,5 which is considerably more expensive than hydrogen and produces a gaseous reaction product, CO2.† The article does not include use of other nongaseous reducing agents,7 which are far more expensive than CO. Also, notes on the history, engineering design, and performance of commercial plants have been given elsewhere.&apos; It will be shown that a pure metal can be precipitated by reduction with hydrogen from solutions obtained by commercial leaching methods when the solution composition is controlled and proper acidity, proper metal ion concentration through controlled complex formation and hydrolysis, and adequate agitation for suspension of metal and for transfer of reducing gas are maintained. Reasonable temperatures and pressures are used which are less excessive than those used by previous workers, although they are maintained at above equilibrium values because of process kinetics.&apos; It has also been found necessary to induce nuclea-tion and to control growth and agglomeration in order to get a powder product of suitable physical properties. Review of the Literature Muller, Schlecht, and Schubardt of I. G. Farben10 claimed a successive reduction of silver, copper, nickel, cobalt, and zinc from ammoniacal solution by applying progressively higher temperatures and hydrogen pressures. Metals produced by this technique were not pure, since no attempt was made to adjust the solution composition between the different reductions. It is doubtful that the zinc product contained any metallic zinc. The major contribution to the literature" was made by the Ipatiews,12 who prepared platinum, iridium, copper, nickel, cobalt, lead, tin, arsenic, antimony, and bismuth at often extreme conditions, up to the critical temperature of water (373ºC), at 1500 to 7500 psi, for as long as several days. Even cadmium and zinc were claimed to have been observed in trace quantities precipitated together with basic salts. In the early experiments solutions were not stirred. Extensive formation of oxides and basic salts occurred, probably long before sufficient hydrogen could be supplied in the unstirred liquid to decrease the metal concentration in solution by reduction. The importance of hydrogen pressure was

Jan 1, 1957

By G. A. Beiswenger

The application of the law of supply and demand to the sale of crude oil is generally conceded, but the motives underlying the buyer&apos;s (refiner&apos;s) demands are not always obvious to the seller (producer). In some cases this obscurity has led to the conclusion that the refiner may be unnecessarily particular when he selects one crude and rejects another. This preference, however, is very largely the reflection of the refiner&apos;s product demands and the quality of the stocks obtainable from the selected crude. The purpose of this paper is to point out critical characteristies of the major classes of refined products and to show how crudes vary in their suitability for such products. With relatively few exceptions, available processing methods and addition agents make it theoretically possible to produce any type of refined product from any crude source, although it may not be economically sound to do so. The widespread application of thermal cracking for converting higher boiling stocks into gasoline is well known. More recently cracking and refining in the presence of catalysts9 have been developed, as well as various processes for polymerizing lighter hydrocarbons into gasolines having desirable characteristics.6 For several years, selective solvents have been applied commercially to refining inferior quality kerosene, Diesel fuel and lubricating oil distillates.3 Improved methods for refining lubricating oils from crude residual4 formerly suitable only for fuel, are now in use and a number of special solvent processes are available for dewaxing lubricating oils to low pour point.5 These improved refining methods have been developed not only to meet the demand for improved product quality but also to enable the refiner to obtain quality products from crude sources that would not yield such products by the older refining methods. In many cases, the utilization of these modern refining tools necessitates an appreciable expenditure for equipment as well as added manufacturing costs, and their application therefore must be justified economically. Despite the availability of such tools, the added processing costs involved and yields obtainable may render their application entirely impractical. To illustrate this point, inspections of typical cuts from various crudes

Jan 1, 1940

By G. A. Beiswenger

The application of the law of supply and demand to the sale of crude oil is generally conceded, but the motives underlying the buyer&apos;s (refiner&apos;s) demands are not always obvious to the seller (producer). In some cases this obscurity has led to the conclusion that the refiner may be unnecessarily particular when he selects one crude and rejects another. This preference, however, is very largely the reflection of the refiner&apos;s product demands and the quality of the stocks obtainable from the selected crude. The purpose of this paper is to point out critical characteristics of the major classes of refined products and to show how crudes vary in their suitability for such products. With relatively few exceptions, available processing methods and addition agents make it theoretically possible to produce any type of refined product from any crude source, although it may not be economi-cally sound to do so. The widespread application of thermal cracking for converting higher boiling stocks into gasoline is well known. More recently cracking and refining in the presence of catalysts9 have been developed, as well as various processes for polymerizing lighter hydro-carbons into gasolines having desirable characteristics.6 For several years, selective solvents have been applied commercially to refining inferior quality kerosene, Diesel fuel and lubricating oil distillates .3 Improved methods for refining lubricating oils from crude residua,4 formerly suitable only for fuel, are now in use and a number of special solvent processes are available for dewaxing lubricating oils to low pour point.5 These improved refining methods have been developed not only to meet the demand for improved product quality but also to enable the refiner to obtain quality products from crude sources that would not yield such products by the older refining methods. In many cases, the utilization of these modern refining tools necessi-tates an appreciable expenditure for equipment as well as added manufac-turing costs, and their application therefore must be justified economically. Despite the availability of such tools, the added processing costs involved and yields obtainable may render their application entirely impractical. To illustrate this point, inspections of typical cuts from various crudes

Jan 1, 1940

By F. W. Jr. Sperr

THE byproduct coke oven is the most important artificial source of fuels for metals melting. Its products are solid, liquid, and gaseous in form. The amount of coke and primary byproducts obtained per ton of coal varies with the nature of the coal. The following represents the results obtained in many plants: Metallurgical coke (over 3/4 in.) 69 per cent. of coal Domestic coke (1/2 to 3/4 in.) 2 per cent. of coal Breeze (under 1/2 in.) 4 per cent. of coal Surplus gas, cubic feet per net ton 6600 Gas for heating ovens, cubic feet per net ton 4400 Tar, gallons per net ton 9 Ammonium sulfate, pounds per net ton 25 Benzols, gallons per net ton 4 All of these products, except ammonium sulfate, have important fuel value. Part or all of the metallurgical coke may be crushed or screened to furnish additional domestic coke. If producer gas is used, there will be a surplus of 11,000 cu. ft. of coke-oven gas per net ton of coal. The use of coke in the metallurgical industries has been retarded by the mental attitude of writers who disregard the dependence of coke quality on the conditions of its manufacture. Terms like "byproduct coke,"&apos; "beehive coke," "48-hour coke," and "72-hour coke" are only generally descriptive and tell nothing of the coke quality. For example, one writer1 stated that in brass-foundry practice, Connellsville coke is considered much superior to byproduct coke on account of the high sulfur content of the latter. Another2 says, "At equal prices for hard Connellsville coke and for byproduct coke at the foundry door, the hard coke is unquestionably cheaper. It will melt more metal per ton than the byproduct coke and requires less labor, as the byproduct coke is less dense and burns faster, thus requiring more frequent firing." A little study of the conditions under which coke is manufactured will show the error in mak-

Jan 10, 1920

US 4,185,872-In the solution mining of uranium values from a subterranean uranium ore deposit, a lixiviant comprising sodium sulfate or other alkali metal sulfate and optionally minor proportions of an alkali metal carbonate or bicarbonate and an alkali metal hypochlorite is introduced into the ore to solubilize uranium therein. The pregnant lixiviant is recovered for processing. E.T. Habib, Jr., assigned to Mobil Oil Corp. Jan. 29, 1980. 5 pp (299-4). Filed- 8-18-78 (934,933).

Jan 1, 1982

By L. A. Tarshis, H. E. Cline

A stability criterion for a lamellar eutectic interface was derived previously1 assuming that the wavelength, A,. of the perturbation which grows most rapidly is much larger than the lamellar spacing. A. This assumption was required to permit averaging of both the interface temperature and composition over the complicated geometry of a lamellae. If this assumption is invalid, as has been suggested.2,3 then the problem becomes too complicated to solve completely. The first of these analyses1 did not calculate the wavelength. A,. of the initially unstable perturbation. whereas the more recent analysis.&apos; which led to a contradiction of this assumption. did not include one of the key factors for determining this wavelength. To rigorously determine the wavelength, the effect of the curvature of the perturbed interface (not considered by either of the above treatments) must be included. By omitting this term, one would be led to an incorrect conclusion regarding the magnitude of A,. but to an accurate criterion for stability as evidenced by the excellent agreement with experimental observations.&apos; In the case of single-phase alloys. the critical wavelength. A,. for instability can be calculated from the Mullins and Sekerka4 (M.S.) analysis which includes the effects of capillarity. In the following discussion, the M.S. analysis is applied to lamellar eutectics and the critical wavelengths calculated for reasonable growth conditions in Pb-Sn eutectic alloys. In order to apply the M.S. analysis to eutectics. one may substitute i) the effective liquidus slope.1 m*. for the single-phase liquidus slope and ii) the ratio of the bulk alloy composition. C,. to the average interface composition in the liquid (Ci = CE where CE is the equilibrium eutectic composition) for the distribution coefficient to give:

Jan 1, 1970

By Edwin C. Holden

In making the original estimates for a report recommending the cyanidation of Ymir stamp-mill tailings, the writer was unable to find in any of the standard works on cyanide-practice certain data applicable to the local conditions; nor has he as yet seen quite the same practice recorded in the rapidly growing literature of cyanidation. To present these figures, together with a few novel features of local practice, the present paper is offered. The ore treated is obtained from a fissure-vein of steep dip, occurring in a slate country. The ore-body is lenticular in plan, swelling from 4 ft. in width at one end to a maximum of 42 ft., and tapering irregularly to less than 18 in., where payvalues cease. In the wider portions of the fissure the ore is mixed with more or less horse-matter from the walls. The clean ore is white, massive quartz, with from 8 to 12 per cent of sulphurets; the latter being pyrite, sphalerite and galena, the predominance being in the order given. The precious metal tenor is variable, the gold more closely following the pyrite, the silver the galena. The present mill-supply is practically all from below the oxidized zone. The unavoidable admixture of horse-matter and stope-filling with the ore as mined, affects more or less the character of the mill-feed, which sometimes contains from 10 to 25 per cent of slate. During the last three months of 1902, the mill-feed carried 0.3977 oz. gold and 1.903 oz. silver per ton of 2,000 lb., 2.65 per cent lead and 2.92 per cent zinc. The iron, unfortunately, was not determined. The Ymir mill and mine have been fully described elsewhere;* suffice it to say of the milling that the crushed ore,

Jan 1, 1904